# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof Xue Si-Jia' _publ_contact_author_email SJXUE@SOHU.COM _publ_section_title ; A New Class of Functionalized Polyoxometalates: Synthesis, Structure and Preliminary Antitumor Activity Studies of Three Arylimido Substituted Hexamolybdate Bearing a Strong Electron-withdrawing Nitro Group, (Bu4N)2[Mo6O18 (?NAr)] (Ar =3-NO2-C6H4? 2-CH3-4-NO2-C6H3? 2-CH3-5-NO2-C6H3) ; loop_ _publ_author_name 'Xue Si-Jia' 'Wangdong Bian' 'Zhijuan Cai' 'An Chai' 'Jian Shen' ; Yongge Wei ; 'Changsheng Xiang' # Attachment '061114a.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 671418' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H76 Mo6 N4 O20' _chemical_formula_weight 1484.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.8273(17) _cell_length_b 17.3291(17) _cell_length_c 19.685(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.057(2) _cell_angle_gamma 90.00 _cell_volume 5739.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 7897 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 19.77 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 1.339 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7755 _exptl_absorpt_correction_T_max 0.8777 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39154 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10083 _reflns_number_gt 5530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The benzene ring of the imido group and all the 8 butyl groups was refined with similarity restraint using the "SAME" instruction. All the carbon atoms in the two tetrabutylammonium was refined with both "SIMU" and "ISOR" instructions to make them have acceptable Uijs. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+17.0986P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10083 _refine_ls_number_parameters 613 _refine_ls_number_restraints 566 _refine_ls_R_factor_all 0.1351 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1412 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.24847(7) 0.60906(7) 0.22190(5) 0.1134(4) Uani 1 1 d . . . Mo2 Mo 0.25394(6) 0.76451(6) 0.31466(6) 0.1012(4) Uani 1 1 d . . . Mo3 Mo 0.11466(5) 0.63372(5) 0.33754(5) 0.0805(3) Uani 1 1 d . . . Mo4 Mo 0.25914(6) 0.65505(6) 0.45268(5) 0.0931(3) Uani 1 1 d . . . Mo5 Mo 0.25310(5) 0.49891(5) 0.35656(5) 0.0887(3) Uani 1 1 d . . . Mo6 Mo 0.39279(6) 0.63015(6) 0.33347(7) 0.1140(4) Uani 1 1 d . . . O1 O 0.2544(3) 0.6313(3) 0.3341(3) 0.0715(16) Uani 1 1 d . . . O2 O 0.1352(4) 0.6114(4) 0.2440(3) 0.100(2) Uani 1 1 d . . . O3 O 0.2479(4) 0.7187(4) 0.2251(3) 0.115(3) Uani 1 1 d . . . O4 O 0.2503(4) 0.5045(4) 0.2611(4) 0.110(2) Uani 1 1 d . . . O5 O 0.2517(5) 0.8598(4) 0.2997(5) 0.145(3) Uani 1 1 d . . . O6 O 0.1402(4) 0.7384(4) 0.3204(3) 0.090(2) Uani 1 1 d . . . O7 O 0.2575(4) 0.7578(4) 0.4112(4) 0.102(2) Uani 1 1 d . . . O8 O 0.3653(4) 0.7393(4) 0.3168(4) 0.124(3) Uani 1 1 d . . . O9 O 0.0148(3) 0.6334(4) 0.3400(4) 0.108(2) Uani 1 1 d . . . O10 O 0.1475(4) 0.6513(3) 0.4315(3) 0.0846(19) Uani 1 1 d . . . O11 O 0.1430(3) 0.5249(3) 0.3562(3) 0.0875(19) Uani 1 1 d . . . O12 O 0.2634(5) 0.6729(5) 0.5356(4) 0.134(3) Uani 1 1 d . . . O13 O 0.2593(4) 0.5459(4) 0.4462(3) 0.097(2) Uani 1 1 d . . . O14 O 0.3689(4) 0.6529(4) 0.4274(4) 0.111(2) Uani 1 1 d . . . O15 O 0.2536(4) 0.4027(4) 0.3737(4) 0.125(3) Uani 1 1 d . . . O16 O 0.3671(4) 0.5249(4) 0.3516(3) 0.100(2) Uani 1 1 d . . . O17 O 0.4930(4) 0.6313(5) 0.3320(5) 0.162(4) Uani 1 1 d . . . O18 O 0.3636(5) 0.6123(5) 0.2405(4) 0.128(3) Uani 1 1 d . . . N1 N 0.2444(7) 0.5843(7) 0.1380(5) 0.148(4) Uani 1 1 d . . . C6 C 0.2153(11) 0.4709(9) 0.0685(7) 0.251(8) Uani 1 1 d DU . . H6 H 0.1995 0.4446 0.1072 0.301 Uiso 1 1 calc R . . C1 C 0.2439(10) 0.5467(9) 0.0738(6) 0.219(7) Uani 1 1 d DU . . C2 C 0.2743(9) 0.5830(8) 0.0173(7) 0.273(9) Uani 1 1 d DU . . H2 H 0.2945 0.6328 0.0210 0.328 Uiso 1 1 calc R . . C3 C 0.2746(12) 0.5449(10) -0.0454(7) 0.310(9) Uani 1 1 d DU . . H3 H 0.2960 0.5690 -0.0831 0.372 Uiso 1 1 calc R . . C4 C 0.2428(13) 0.4707(11) -0.0513(7) 0.316(9) Uani 1 1 d DU . . H4 H 0.2430 0.4451 -0.0928 0.380 Uiso 1 1 calc R . . C5 C 0.2108(15) 0.4353(11) 0.0057(7) 0.296(9) Uani 1 1 d DU . . N2 N 0.1822(19) 0.3580(14) 0.0004(9) 0.362(11) Uani 1 1 d DU . . O19 O 0.1843(18) 0.3244(12) -0.0563(13) 0.510(16) Uani 1 1 d DU . . O20 O 0.1566(17) 0.3251(11) 0.0530(12) 0.415(12) Uani 1 1 d DU . . N3 N 0.9734(5) 0.3600(4) 0.3390(4) 0.082(2) Uani 1 1 d . . . C7 C 0.9353(7) 0.3853(6) 0.2703(5) 0.101(3) Uani 1 1 d D . . H7A H 0.9330 0.3410 0.2403 0.122 Uiso 1 1 calc R . . H7B H 0.8811 0.4017 0.2782 0.122 Uiso 1 1 calc R . . C8 C 0.9781(7) 0.4495(6) 0.2351(5) 0.115(4) Uani 1 1 d D . . H8A H 1.0296 0.4313 0.2205 0.138 Uiso 1 1 calc R . . H8B H 0.9868 0.4920 0.2665 0.138 Uiso 1 1 calc R . . C9 C 0.9296(9) 0.4775(8) 0.1735(6) 0.179(7) Uani 1 1 d D . . H9A H 0.9162 0.4339 0.1447 0.215 Uiso 1 1 calc R . . H9B H 0.8804 0.5004 0.1887 0.215 Uiso 1 1 calc R . . C10 C 0.9742(10) 0.5354(9) 0.1335(7) 0.196(8) Uani 1 1 d D . . H10A H 0.9418 0.5525 0.0958 0.294 Uiso 1 1 calc R . . H10B H 1.0220 0.5124 0.1171 0.294 Uiso 1 1 calc R . . H10C H 0.9875 0.5787 0.1620 0.294 Uiso 1 1 calc R . . C11 C 0.9737(6) 0.4273(5) 0.3887(5) 0.092(3) Uani 1 1 d D . . H11A H 0.9898 0.4076 0.4330 0.111 Uiso 1 1 calc R . . H11B H 1.0142 0.4634 0.3747 0.111 Uiso 1 1 calc R . . C12 C 0.8974(7) 0.4717(6) 0.3970(5) 0.101(3) Uani 1 1 d D . . H12A H 0.8547 0.4360 0.4067 0.121 Uiso 1 1 calc R . . H12B H 0.8841 0.4982 0.3549 0.121 Uiso 1 1 calc R . . C13 C 0.9048(7) 0.5308(6) 0.4548(5) 0.115(4) Uani 1 1 d D . . H13A H 0.9051 0.5036 0.4979 0.138 Uiso 1 1 calc R . . H13B H 0.9553 0.5574 0.4512 0.138 Uiso 1 1 calc R . . C14 C 0.8402(9) 0.5885(7) 0.4546(7) 0.170(6) Uani 1 1 d D . . H14A H 0.8492 0.6246 0.4910 0.255 Uiso 1 1 calc R . . H14B H 0.7902 0.5630 0.4606 0.255 Uiso 1 1 calc R . . H14C H 0.8393 0.6156 0.4120 0.255 Uiso 1 1 calc R . . C15 C 0.9238(6) 0.2926(5) 0.3656(5) 0.093(3) Uani 1 1 d D . . H15A H 0.8698 0.3107 0.3717 0.112 Uiso 1 1 calc R . . H15B H 0.9219 0.2528 0.3310 0.112 Uiso 1 1 calc R . . C16 C 0.9519(7) 0.2570(6) 0.4305(5) 0.111(4) Uani 1 1 d D . . H16A H 0.9506 0.2955 0.4661 0.133 Uiso 1 1 calc R . . H16B H 1.0067 0.2408 0.4256 0.133 Uiso 1 1 calc R . . C17 C 0.9027(8) 0.1881(6) 0.4516(6) 0.135(5) Uani 1 1 d D . . H17A H 0.8478 0.2043 0.4556 0.161 Uiso 1 1 calc R . . H17B H 0.9046 0.1495 0.4160 0.161 Uiso 1 1 calc R . . C18 C 0.9290(10) 0.1521(7) 0.5166(6) 0.176(7) Uani 1 1 d D . . H18A H 0.8946 0.1097 0.5270 0.264 Uiso 1 1 calc R . . H18B H 0.9270 0.1897 0.5524 0.264 Uiso 1 1 calc R . . H18C H 0.9825 0.1336 0.5126 0.264 Uiso 1 1 calc R . . C19 C 1.0586(7) 0.3348(6) 0.3302(5) 0.107(4) Uani 1 1 d D . . H19A H 1.0886 0.3787 0.3138 0.128 Uiso 1 1 calc R . . H19B H 1.0805 0.3213 0.3746 0.128 Uiso 1 1 calc R . . C20 C 1.0723(8) 0.2678(7) 0.2827(6) 0.134(5) Uani 1 1 d D . . H20A H 1.0459 0.2771 0.2393 0.160 Uiso 1 1 calc R . . H20B H 1.0509 0.2207 0.3019 0.160 Uiso 1 1 calc R . . C21 C 1.1623(9) 0.2594(11) 0.2731(11) 0.231(10) Uani 1 1 d D . . H21A H 1.1837 0.3094 0.2609 0.278 Uiso 1 1 calc R . . H21B H 1.1866 0.2445 0.3162 0.278 Uiso 1 1 calc R . . C22 C 1.1839(12) 0.2065(17) 0.2244(13) 0.40(2) Uani 1 1 d D . . H22A H 1.2404 0.2081 0.2189 0.599 Uiso 1 1 calc R . . H22B H 1.1578 0.2189 0.1820 0.599 Uiso 1 1 calc R . . H22C H 1.1684 0.1557 0.2384 0.599 Uiso 1 1 calc R . . N4 N 0.4949(7) 0.3229(8) 0.3399(7) 0.220(5) Uani 1 1 d DU . . C23 C 0.4452(9) 0.3497(10) 0.2758(7) 0.217(6) Uani 1 1 d DU . . H23A H 0.3912 0.3338 0.2853 0.260 Uiso 1 1 calc R . . H23B H 0.4450 0.4056 0.2788 0.260 Uiso 1 1 calc R . . C24 C 0.4537(14) 0.3345(15) 0.2062(9) 0.287(9) Uani 1 1 d DU . . H24A H 0.4535 0.2790 0.1997 0.344 Uiso 1 1 calc R . . H24B H 0.5053 0.3533 0.1926 0.344 Uiso 1 1 calc R . . C25 C 0.3916(14) 0.3689(17) 0.1591(10) 0.307(11) Uani 1 1 d DU . . H25A H 0.3449 0.3362 0.1560 0.369 Uiso 1 1 calc R . . H25B H 0.3759 0.4198 0.1745 0.369 Uiso 1 1 calc R . . C26 C 0.431(2) 0.373(2) 0.0945(13) 0.48(2) Uani 1 1 d DU . . H26A H 0.4027 0.4084 0.0651 0.721 Uiso 1 1 calc R . . H26B H 0.4318 0.3230 0.0740 0.721 Uiso 1 1 calc R . . H26C H 0.4844 0.3913 0.1016 0.721 Uiso 1 1 calc R . . C27 C 0.5743(9) 0.3574(11) 0.3387(11) 0.296(9) Uani 1 1 d DU . . H27A H 0.5999 0.3460 0.3821 0.356 Uiso 1 1 calc R . . H27B H 0.6039 0.3300 0.3044 0.356 Uiso 1 1 calc R . . C28 C 0.5850(12) 0.4392(12) 0.3262(14) 0.322(11) Uani 1 1 d DU . . H28A H 0.5526 0.4678 0.3578 0.387 Uiso 1 1 calc R . . H28B H 0.5656 0.4509 0.2807 0.387 Uiso 1 1 calc R . . C29 C 0.6708(12) 0.4676(15) 0.3333(13) 0.306(11) Uani 1 1 d DU . . H29A H 0.6819 0.4836 0.3798 0.368 Uiso 1 1 calc R . . H29B H 0.7073 0.4265 0.3220 0.368 Uiso 1 1 calc R . . C30 C 0.6811(13) 0.5325(13) 0.2874(12) 0.305(13) Uani 1 1 d DU . . H30A H 0.7351 0.5504 0.2904 0.457 Uiso 1 1 calc R . . H30B H 0.6459 0.5735 0.2997 0.457 Uiso 1 1 calc R . . H30C H 0.6692 0.5164 0.2417 0.457 Uiso 1 1 calc R . . C31 C 0.4466(9) 0.3491(10) 0.3987(7) 0.243(7) Uani 1 1 d DU . . H31A H 0.4339 0.4030 0.3910 0.291 Uiso 1 1 calc R . . H31B H 0.3967 0.3210 0.3963 0.291 Uiso 1 1 calc R . . C32 C 0.4763(13) 0.3428(16) 0.4676(10) 0.344(11) Uani 1 1 d DU . . H32A H 0.5250 0.3724 0.4725 0.412 Uiso 1 1 calc R . . H32B H 0.4886 0.2892 0.4775 0.412 Uiso 1 1 calc R . . C33 C 0.4137(18) 0.3731(17) 0.5194(12) 0.402(15) Uani 1 1 d DU . . H33A H 0.4382 0.3779 0.5642 0.482 Uiso 1 1 calc R . . H33B H 0.3947 0.4236 0.5054 0.482 Uiso 1 1 calc R . . C34 C 0.3457(16) 0.3174(18) 0.5215(17) 0.455(19) Uani 1 1 d DU . . H34A H 0.3053 0.3375 0.5504 0.682 Uiso 1 1 calc R . . H34B H 0.3642 0.2688 0.5391 0.682 Uiso 1 1 calc R . . H34C H 0.3242 0.3102 0.4765 0.682 Uiso 1 1 calc R . . C35 C 0.4966(13) 0.2354(9) 0.3370(10) 0.320(9) Uani 1 1 d DU . . H35A H 0.4428 0.2153 0.3356 0.383 Uiso 1 1 calc R . . H35B H 0.5233 0.2186 0.2963 0.383 Uiso 1 1 calc R . . C36 C 0.5379(16) 0.2077(15) 0.3957(12) 0.379(13) Uani 1 1 d DU . . H36A H 0.5143 0.2330 0.4344 0.455 Uiso 1 1 calc R . . H36B H 0.5919 0.2268 0.3931 0.455 Uiso 1 1 calc R . . C37 C 0.5441(18) 0.1206(17) 0.414(2) 0.447(16) Uani 1 1 d DU . . H37A H 0.5851 0.0962 0.3872 0.537 Uiso 1 1 calc R . . H37B H 0.5577 0.1144 0.4616 0.537 Uiso 1 1 calc R . . C38 C 0.466(2) 0.0850(19) 0.398(3) 0.60(3) Uani 1 1 d DU . . H38A H 0.4679 0.0310 0.4093 0.901 Uiso 1 1 calc R . . H38B H 0.4532 0.0912 0.3509 0.901 Uiso 1 1 calc R . . H38C H 0.4258 0.1096 0.4248 0.901 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.1249(9) 0.1409(11) 0.0753(7) 0.0075(7) 0.0246(6) 0.0158(8) Mo2 0.0907(7) 0.0810(7) 0.1326(10) 0.0306(6) 0.0187(6) -0.0060(6) Mo3 0.0635(5) 0.0874(7) 0.0907(7) 0.0191(5) 0.0043(5) 0.0001(5) Mo4 0.0957(7) 0.1009(8) 0.0821(7) -0.0002(6) -0.0101(5) 0.0070(6) Mo5 0.0784(6) 0.0740(6) 0.1137(8) 0.0083(6) 0.0043(5) 0.0032(5) Mo6 0.0622(6) 0.1105(9) 0.1698(12) 0.0160(8) 0.0192(7) -0.0021(6) O1 0.057(3) 0.078(4) 0.080(4) 0.019(3) 0.010(3) 0.000(3) O2 0.093(5) 0.123(6) 0.084(5) 0.009(4) -0.006(4) 0.002(4) O3 0.119(6) 0.128(6) 0.099(5) 0.031(5) 0.045(5) 0.010(5) O4 0.111(6) 0.099(5) 0.122(6) -0.018(5) 0.018(5) 0.012(4) O5 0.132(7) 0.094(6) 0.208(9) 0.052(6) 0.014(6) -0.020(5) O6 0.076(4) 0.097(5) 0.098(5) 0.019(4) 0.006(4) 0.015(4) O7 0.097(5) 0.086(5) 0.122(6) -0.020(4) -0.007(4) 0.001(4) O8 0.075(5) 0.109(6) 0.189(8) 0.022(5) 0.029(5) -0.025(4) O9 0.050(4) 0.137(6) 0.136(6) 0.030(5) 0.007(4) -0.002(4) O10 0.085(4) 0.090(5) 0.080(4) 0.013(4) 0.026(4) 0.019(4) O11 0.074(4) 0.081(4) 0.108(5) 0.015(4) 0.002(4) -0.011(3) O12 0.156(7) 0.148(7) 0.098(6) -0.020(5) -0.023(5) 0.023(6) O13 0.096(5) 0.089(5) 0.104(5) 0.027(4) -0.008(4) 0.010(4) O14 0.079(5) 0.101(5) 0.152(7) -0.013(5) -0.026(5) -0.006(4) O15 0.119(6) 0.079(5) 0.178(8) 0.009(5) -0.003(6) 0.017(4) O16 0.076(5) 0.100(5) 0.124(6) -0.001(4) 0.005(4) 0.018(4) O17 0.061(5) 0.155(8) 0.270(11) 0.010(7) 0.022(6) -0.001(5) O18 0.116(6) 0.148(7) 0.122(6) 0.015(5) 0.059(5) 0.012(5) N1 0.187(11) 0.180(11) 0.078(7) 0.013(7) 0.033(7) 0.054(9) C6 0.32(2) 0.236(15) 0.191(13) 0.015(12) -0.060(15) 0.130(16) C1 0.34(2) 0.216(14) 0.101(9) 0.041(10) 0.006(12) 0.150(15) C2 0.46(2) 0.268(15) 0.096(10) 0.044(10) 0.060(14) 0.190(15) C3 0.48(2) 0.34(2) 0.112(10) 0.016(12) 0.042(16) 0.199(19) C4 0.40(2) 0.36(2) 0.184(14) -0.030(14) -0.061(16) 0.204(19) C5 0.38(2) 0.274(16) 0.232(16) -0.021(13) -0.093(18) 0.141(17) N2 0.43(3) 0.300(19) 0.35(2) -0.076(15) -0.14(2) 0.13(2) O19 0.64(4) 0.44(2) 0.44(3) -0.22(2) -0.20(3) 0.18(2) O20 0.43(3) 0.32(2) 0.49(3) -0.04(2) -0.12(3) -0.04(2) N3 0.089(6) 0.076(6) 0.079(6) -0.011(5) 0.006(5) -0.014(5) C7 0.123(9) 0.108(9) 0.073(7) -0.005(7) 0.005(7) -0.025(7) C8 0.164(12) 0.103(9) 0.079(8) 0.006(7) 0.009(8) -0.037(8) C9 0.26(2) 0.176(15) 0.098(10) 0.051(10) 0.000(12) -0.081(14) C10 0.27(2) 0.200(17) 0.118(12) 0.039(11) -0.028(12) -0.079(15) C11 0.126(10) 0.069(7) 0.081(7) -0.022(6) -0.003(7) -0.023(7) C12 0.126(10) 0.086(8) 0.091(8) -0.011(7) 0.004(7) -0.008(7) C13 0.162(12) 0.092(9) 0.090(8) -0.008(7) 0.029(8) -0.003(8) C14 0.26(2) 0.109(11) 0.143(13) 0.001(9) 0.036(12) 0.045(12) C15 0.116(9) 0.064(7) 0.099(8) -0.003(6) 0.011(7) -0.028(6) C16 0.144(11) 0.098(9) 0.091(9) 0.010(7) 0.024(8) -0.014(8) C17 0.187(14) 0.082(9) 0.137(12) 0.007(8) 0.039(10) -0.013(9) C18 0.28(2) 0.129(12) 0.122(12) 0.047(10) 0.025(12) 0.029(12) C19 0.110(10) 0.113(9) 0.098(8) -0.016(7) 0.017(7) -0.023(8) C20 0.145(13) 0.131(11) 0.126(11) -0.026(9) 0.029(9) 0.010(9) C21 0.161(18) 0.26(2) 0.27(2) -0.147(19) 0.040(16) 0.038(15) C22 0.19(2) 0.64(6) 0.37(4) -0.24(4) 0.05(2) -0.04(3) N4 0.147(10) 0.241(11) 0.272(12) -0.064(12) 0.034(10) 0.072(9) C23 0.183(14) 0.254(15) 0.213(11) -0.079(13) 0.011(11) -0.059(13) C24 0.28(2) 0.33(2) 0.252(12) -0.084(18) 0.040(16) 0.007(19) C25 0.32(3) 0.40(3) 0.203(15) -0.08(2) 0.014(15) 0.01(2) C26 0.53(5) 0.60(5) 0.31(2) 0.09(3) 0.13(2) 0.07(4) C27 0.183(12) 0.359(19) 0.35(2) -0.05(2) -0.048(12) 0.044(14) C28 0.221(17) 0.38(2) 0.36(2) -0.05(2) -0.090(18) -0.059(16) C29 0.171(16) 0.44(3) 0.31(3) 0.01(2) -0.03(2) 0.000(16) C30 0.25(2) 0.32(3) 0.35(3) -0.05(2) 0.09(2) 0.045(17) C31 0.220(15) 0.306(17) 0.200(11) -0.103(15) -0.036(11) 0.156(14) C32 0.34(2) 0.46(3) 0.231(13) -0.10(2) -0.085(15) 0.21(2) C33 0.43(3) 0.60(3) 0.180(14) -0.10(2) -0.057(19) 0.24(3) C34 0.39(3) 0.60(4) 0.37(4) 0.06(3) 0.00(3) 0.27(3) C35 0.33(2) 0.248(12) 0.39(2) -0.094(14) 0.11(2) 0.112(14) C36 0.40(3) 0.32(2) 0.43(3) 0.02(2) 0.16(2) 0.18(2) C37 0.49(4) 0.31(2) 0.55(3) 0.04(3) 0.20(3) 0.13(3) C38 0.62(5) 0.49(4) 0.70(5) -0.18(4) 0.28(5) -0.05(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.707(10) . ? Mo1 O3 1.901(7) . ? Mo1 O2 1.964(7) . ? Mo1 O18 1.966(8) . ? Mo1 O4 1.969(7) . ? Mo1 O1 2.242(6) . ? Mo2 O5 1.678(7) . ? Mo2 O7 1.904(7) . ? Mo2 O8 1.923(7) . ? Mo2 O3 1.935(7) . ? Mo2 O6 1.973(6) . ? Mo2 O1 2.339(6) . ? Mo3 O9 1.683(6) . ? Mo3 O6 1.896(6) . ? Mo3 O2 1.919(6) . ? Mo3 O10 1.944(6) . ? Mo3 O11 1.977(6) . ? Mo3 O1 2.354(5) . ? Mo4 O12 1.661(7) . ? Mo4 O13 1.895(6) . ? Mo4 O10 1.919(6) . ? Mo4 O14 1.922(7) . ? Mo4 O7 1.959(7) . ? Mo4 O1 2.370(6) . ? Mo5 O15 1.701(7) . ? Mo5 O4 1.882(7) . ? Mo5 O11 1.907(6) . ? Mo5 O13 1.945(7) . ? Mo5 O16 1.975(6) . ? Mo5 O1 2.337(5) . ? Mo6 O17 1.687(7) . ? Mo6 O16 1.909(7) . ? Mo6 O18 1.911(8) . ? Mo6 O14 1.940(8) . ? Mo6 O8 1.974(7) . ? Mo6 O1 2.329(5) . ? N1 C1 1.421(14) . ? C6 C5 1.383(7) . ? C6 C1 1.402(9) . ? C6 H6 0.9300 . ? C1 C2 1.384(7) . ? C2 C3 1.399(9) . ? C2 H2 0.9300 . ? C3 C4 1.398(9) . ? C3 H3 0.9300 . ? C4 C5 1.395(9) . ? C4 H4 0.9300 . ? C5 N2 1.426(18) . ? N2 O19 1.260(12) . ? N2 O20 1.266(12) . ? N3 C19 1.513(12) . ? N3 C11 1.522(10) . ? N3 C15 1.532(10) . ? N3 C7 1.550(11) . ? C7 C8 1.502(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.529(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.486(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.508(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.533(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.477(12) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.488(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.515(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.485(12) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.512(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.536(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.380(14) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? N4 C27 1.465(14) . ? N4 C31 1.497(13) . ? N4 C35 1.517(14) . ? N4 C23 1.571(14) . ? C23 C24 1.405(14) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.507(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.447(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.451(15) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.530(15) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.455(15) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.441(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.570(15) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.498(17) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.421(15) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.553(15) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.481(17) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 O3 106.4(4) . . ? N1 Mo1 O2 101.4(4) . . ? O3 Mo1 O2 88.1(3) . . ? N1 Mo1 O18 102.1(4) . . ? O3 Mo1 O18 88.3(3) . . ? O2 Mo1 O18 156.3(3) . . ? N1 Mo1 O4 98.5(4) . . ? O3 Mo1 O4 155.1(3) . . ? O2 Mo1 O4 86.6(3) . . ? O18 Mo1 O4 86.8(3) . . ? N1 Mo1 O1 175.4(4) . . ? O3 Mo1 O1 78.2(3) . . ? O2 Mo1 O1 78.7(2) . . ? O18 Mo1 O1 77.6(3) . . ? O4 Mo1 O1 76.9(2) . . ? O5 Mo2 O7 103.6(4) . . ? O5 Mo2 O8 104.2(3) . . ? O7 Mo2 O8 87.2(3) . . ? O5 Mo2 O3 104.1(4) . . ? O7 Mo2 O3 152.2(3) . . ? O8 Mo2 O3 87.8(3) . . ? O5 Mo2 O6 102.6(3) . . ? O7 Mo2 O6 86.7(3) . . ? O8 Mo2 O6 153.2(3) . . ? O3 Mo2 O6 85.6(3) . . ? O5 Mo2 O1 178.7(3) . . ? O7 Mo2 O1 77.1(2) . . ? O8 Mo2 O1 76.8(2) . . ? O3 Mo2 O1 75.2(2) . . ? O6 Mo2 O1 76.4(2) . . ? O9 Mo3 O6 103.8(3) . . ? O9 Mo3 O2 102.9(3) . . ? O6 Mo3 O2 88.6(3) . . ? O9 Mo3 O10 103.9(3) . . ? O6 Mo3 O10 87.6(3) . . ? O2 Mo3 O10 153.0(3) . . ? O9 Mo3 O11 103.2(3) . . ? O6 Mo3 O11 153.0(2) . . ? O2 Mo3 O11 86.5(3) . . ? O10 Mo3 O11 84.8(3) . . ? O9 Mo3 O1 178.8(3) . . ? O6 Mo3 O1 77.4(2) . . ? O2 Mo3 O1 76.8(2) . . ? O10 Mo3 O1 76.4(2) . . ? O11 Mo3 O1 75.6(2) . . ? O12 Mo4 O13 104.6(3) . . ? O12 Mo4 O10 104.1(3) . . ? O13 Mo4 O10 87.4(3) . . ? O12 Mo4 O14 103.5(4) . . ? O13 Mo4 O14 87.7(3) . . ? O10 Mo4 O14 152.3(3) . . ? O12 Mo4 O7 103.9(3) . . ? O13 Mo4 O7 151.5(3) . . ? O10 Mo4 O7 86.2(3) . . ? O14 Mo4 O7 85.2(3) . . ? O12 Mo4 O1 179.1(4) . . ? O13 Mo4 O1 76.2(2) . . ? O10 Mo4 O1 76.4(2) . . ? O14 Mo4 O1 75.9(3) . . ? O7 Mo4 O1 75.4(2) . . ? O15 Mo5 O4 104.4(4) . . ? O15 Mo5 O11 103.5(3) . . ? O4 Mo5 O11 88.7(3) . . ? O15 Mo5 O13 103.4(3) . . ? O4 Mo5 O13 152.2(3) . . ? O11 Mo5 O13 86.6(3) . . ? O15 Mo5 O16 103.4(3) . . ? O4 Mo5 O16 86.8(3) . . ? O11 Mo5 O16 153.0(3) . . ? O13 Mo5 O16 85.0(3) . . ? O15 Mo5 O1 179.0(3) . . ? O4 Mo5 O1 76.1(2) . . ? O11 Mo5 O1 77.3(2) . . ? O13 Mo5 O1 76.1(2) . . ? O16 Mo5 O1 75.8(2) . . ? O17 Mo6 O16 104.1(4) . . ? O17 Mo6 O18 103.0(4) . . ? O16 Mo6 O18 88.2(3) . . ? O17 Mo6 O14 103.8(4) . . ? O16 Mo6 O14 88.0(3) . . ? O18 Mo6 O14 153.1(3) . . ? O17 Mo6 O8 102.6(4) . . ? O16 Mo6 O8 153.3(3) . . ? O18 Mo6 O8 86.6(3) . . ? O14 Mo6 O8 84.9(3) . . ? O17 Mo6 O1 178.7(4) . . ? O16 Mo6 O1 77.2(2) . . ? O18 Mo6 O1 76.5(3) . . ? O14 Mo6 O1 76.6(2) . . ? O8 Mo6 O1 76.2(2) . . ? Mo1 O1 Mo6 91.12(19) . . ? Mo1 O1 Mo5 91.0(2) . . ? Mo6 O1 Mo5 90.29(19) . . ? Mo1 O1 Mo2 90.51(19) . . ? Mo6 O1 Mo2 90.46(19) . . ? Mo5 O1 Mo2 178.3(3) . . ? Mo1 O1 Mo3 90.3(2) . . ? Mo6 O1 Mo3 178.6(3) . . ? Mo5 O1 Mo3 89.95(18) . . ? Mo2 O1 Mo3 89.27(19) . . ? Mo1 O1 Mo4 179.4(3) . . ? Mo6 O1 Mo4 89.49(19) . . ? Mo5 O1 Mo4 89.09(18) . . ? Mo2 O1 Mo4 89.4(2) . . ? Mo3 O1 Mo4 89.10(18) . . ? Mo3 O2 Mo1 114.2(3) . . ? Mo1 O3 Mo2 116.1(3) . . ? Mo5 O4 Mo1 116.0(3) . . ? Mo3 O6 Mo2 116.9(3) . . ? Mo2 O7 Mo4 118.1(3) . . ? Mo2 O8 Mo6 116.5(3) . . ? Mo4 O10 Mo3 118.2(3) . . ? Mo5 O11 Mo3 117.2(3) . . ? Mo4 O13 Mo5 118.6(3) . . ? Mo4 O14 Mo6 117.9(3) . . ? Mo6 O16 Mo5 116.8(3) . . ? Mo6 O18 Mo1 114.7(3) . . ? C1 N1 Mo1 167.1(10) . . ? C5 C6 C1 119.9(9) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C2 C1 C6 119.8(8) . . ? C2 C1 N1 120.7(11) . . ? C6 C1 N1 119.5(11) . . ? C1 C2 C3 120.2(8) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 119.9(9) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 119.5(9) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 120.4(9) . . ? C6 C5 N2 119.9(10) . . ? C4 C5 N2 119.2(10) . . ? O19 N2 O20 122(3) . . ? O19 N2 C5 118.9(18) . . ? O20 N2 C5 118.8(17) . . ? C19 N3 C11 107.6(7) . . ? C19 N3 C15 110.1(8) . . ? C11 N3 C15 111.1(7) . . ? C19 N3 C7 111.1(8) . . ? C11 N3 C7 109.9(8) . . ? C15 N3 C7 107.1(7) . . ? C8 C7 N3 114.7(8) . . ? C8 C7 H7A 108.6 . . ? N3 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? N3 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 C9 110.3(9) . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 111.5(11) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N3 117.9(8) . . ? C12 C11 H11A 107.8 . . ? N3 C11 H11A 107.8 . . ? C12 C11 H11B 107.8 . . ? N3 C11 H11B 107.8 . . ? H11A C11 H11B 107.2 . . ? C11 C12 C13 111.4(9) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 113.7(10) . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N3 116.3(8) . . ? C16 C15 H15A 108.2 . . ? N3 C15 H15A 108.2 . . ? C16 C15 H15B 108.2 . . ? N3 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? C15 C16 C17 113.3(9) . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C16 114.3(11) . . ? C18 C17 H17A 108.7 . . ? C16 C17 H17A 108.7 . . ? C18 C17 H17B 108.7 . . ? C16 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N3 116.6(9) . . ? C20 C19 H19A 108.1 . . ? N3 C19 H19A 108.1 . . ? C20 C19 H19B 108.1 . . ? N3 C19 H19B 108.1 . . ? H19A C19 H19B 107.3 . . ? C19 C20 C21 108.1(10) . . ? C19 C20 H20A 110.1 . . ? C21 C20 H20A 110.1 . . ? C19 C20 H20B 110.1 . . ? C21 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? C22 C21 C20 114.9(15) . . ? C22 C21 H21A 108.5 . . ? C20 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? C20 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C27 N4 C31 113.4(11) . . ? C27 N4 C35 112.8(10) . . ? C31 N4 C35 110.1(10) . . ? C27 N4 C23 109.8(10) . . ? C31 N4 C23 104.1(9) . . ? C35 N4 C23 106.0(10) . . ? C24 C23 N4 131.7(16) . . ? C24 C23 H23A 104.3 . . ? N4 C23 H23A 104.3 . . ? C24 C23 H23B 104.3 . . ? N4 C23 H23B 104.3 . . ? H23A C23 H23B 105.6 . . ? C23 C24 C25 116.3(18) . . ? C23 C24 H24A 108.2 . . ? C25 C24 H24A 108.2 . . ? C23 C24 H24B 108.2 . . ? C25 C24 H24B 108.2 . . ? H24A C24 H24B 107.4 . . ? C26 C25 C24 103.7(18) . . ? C26 C25 H25A 111.0 . . ? C24 C25 H25A 111.0 . . ? C26 C25 H25B 111.0 . . ? C24 C25 H25B 111.0 . . ? H25A C25 H25B 109.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N4 121.1(15) . . ? C28 C27 H27A 107.0 . . ? N4 C27 H27A 107.0 . . ? C28 C27 H27B 107.0 . . ? N4 C27 H27B 107.0 . . ? H27A C27 H27B 106.8 . . ? C27 C28 C29 114.8(18) . . ? C27 C28 H28A 108.6 . . ? C29 C28 H28A 108.6 . . ? C27 C28 H28B 108.6 . . ? C29 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? C30 C29 C28 108.4(17) . . ? C30 C29 H29A 110.0 . . ? C28 C29 H29A 110.0 . . ? C30 C29 H29B 110.0 . . ? C28 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N4 121.4(14) . . ? C32 C31 H31A 107.0 . . ? N4 C31 H31A 107.0 . . ? C32 C31 H31B 107.0 . . ? N4 C31 H31B 107.0 . . ? H31A C31 H31B 106.7 . . ? C31 C32 C33 111.1(16) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 108.9(19) . . ? C34 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? C34 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N4 108.5(17) . . ? C36 C35 H35A 110.0 . . ? N4 C35 H35A 110.0 . . ? C36 C35 H35B 110.0 . . ? N4 C35 H35B 110.0 . . ? H35A C35 H35B 108.4 . . ? C35 C36 C37 123.0(19) . . ? C35 C36 H36A 106.6 . . ? C37 C36 H36A 106.6 . . ? C35 C36 H36B 106.6 . . ? C37 C36 H36B 106.6 . . ? H36A C36 H36B 106.5 . . ? C38 C37 C36 107.6(19) . . ? C38 C37 H37A 110.2 . . ? C36 C37 H37A 110.2 . . ? C38 C37 H37B 110.2 . . ? C36 C37 H37B 110.2 . . ? H37A C37 H37B 108.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2 O7 0.93 2.93 3.468(14) 118.0 4_575 C3 H3 O5 0.93 2.71 3.482(17) 141.3 4_575 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.580 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.088 # Attachment '4-MePhNO2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 671419' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H78 Mo6 N4 O20' _chemical_formula_weight 1498.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.6532(9) _cell_length_b 16.7588(9) _cell_length_c 20.2461(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.0320(10) _cell_angle_gamma 90.00 _cell_volume 5649.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 9708 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.90 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 1.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7725 _exptl_absorpt_correction_T_max 0.8759 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53013 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9926 _reflns_number_gt 7439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The benzene ring of the imido group and all the 8 butyl groups was refined with similarity restraint using the "SAME" instruction. All the carbon atoms in the two tetrabutylammonium was refined with both "SIMU" instruction to make them have acceptable Uijs. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0012P)^2^+63.2290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9926 _refine_ls_number_parameters 526 _refine_ls_number_restraints 333 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.1778 _refine_ls_wR_factor_gt 0.1691 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.24800(8) 0.60657(10) 0.22895(6) 0.1130(5) Uani 1 1 d . A . Mo2 Mo 0.25064(6) 0.49530(6) 0.35960(6) 0.0822(3) Uani 1 1 d . A . Mo3 Mo 0.11493(5) 0.63668(7) 0.34087(5) 0.0792(3) Uani 1 1 d . A . Mo4 Mo 0.39335(6) 0.62659(7) 0.33564(7) 0.0957(4) Uani 1 1 d . A . Mo5 Mo 0.26089(6) 0.65617(7) 0.45123(5) 0.0818(3) Uani 1 1 d . A . Mo6 Mo 0.25783(7) 0.76750(7) 0.31792(7) 0.0962(4) Uani 1 1 d . A . C1 C 0.2341(11) 0.5200(11) 0.0940(8) 0.183 Uani 1 1 d DU A 1 C2 C 0.2631(11) 0.5415(11) 0.0334(8) 0.183 Uani 1 1 d DU A 1 C3 C 0.2650(10) 0.4946(11) -0.0206(8) 0.183 Uani 1 1 d DU A 1 H3 H 0.2949 0.5070 -0.0575 0.220 Uiso 1 1 calc R A 1 C4 C 0.2187(10) 0.4265(9) -0.0163(7) 0.183 Uani 1 1 d DU A 1 C5 C 0.1846(10) 0.4017(11) 0.0414(8) 0.183 Uani 1 1 d DU A 1 H5 H 0.1582 0.3529 0.0434 0.220 Uiso 1 1 calc R A 1 C6 C 0.1899(11) 0.4491(11) 0.0954(8) 0.183 Uani 1 1 d DU A 1 H6 H 0.1638 0.4344 0.1338 0.220 Uiso 1 1 calc R A 1 C7 C 0.3175(8) 0.6127(13) 0.0386(9) 0.183 Uani 1 1 d U A 1 H7A H 0.3388 0.6246 -0.0041 0.274 Uiso 1 1 calc R A 1 H7B H 0.3609 0.6013 0.0690 0.274 Uiso 1 1 calc RD A 1 H7C H 0.2878 0.6578 0.0542 0.274 Uiso 1 1 calc R A 1 N2 N 0.2228(8) 0.3676(8) -0.0664(5) 0.183 Uani 1 1 d DU A 1 O19 O 0.1655(7) 0.3149(7) -0.0664(5) 0.183 Uani 1 1 d DU A 1 O20 O 0.2434(7) 0.3929(7) -0.1241(5) 0.183 Uani 1 1 d DU A 1 C8 C 0.4453(11) 0.1592(11) -0.1053(7) 0.166(7) Uani 1 1 d DU . . H8A H 0.3913 0.1807 -0.1094 0.199 Uiso 1 1 calc RD . . H8B H 0.4406 0.1016 -0.1070 0.199 Uiso 1 1 calc R . . C9 C 0.4769(12) 0.1807(14) -0.0392(9) 0.222(7) Uani 1 1 d DU . . H9A H 0.4808 0.2384 -0.0360 0.266 Uiso 1 1 calc R . . H9B H 0.5306 0.1590 -0.0337 0.266 Uiso 1 1 calc R . . C10 C 0.4236(13) 0.1493(14) 0.0174(9) 0.225 Uani 1 1 d DU . . H10A H 0.4200 0.0917 0.0144 0.270 Uiso 1 1 calc R . . H10B H 0.4489 0.1625 0.0595 0.270 Uiso 1 1 calc R . . C11 C 0.3407(10) 0.1839(12) 0.0149(8) 0.225 Uani 1 1 d DU . . H11A H 0.3044 0.1484 0.0366 0.337 Uiso 1 1 calc RD . . H11B H 0.3238 0.1909 -0.0303 0.337 Uiso 1 1 calc RD . . H11C H 0.3408 0.2347 0.0369 0.337 Uiso 1 1 calc RD . . C12 C 0.5767(9) 0.1553(11) -0.1626(10) 0.155(7) Uani 1 1 d D . . H12A H 0.6067 0.1806 -0.1974 0.186 Uiso 1 1 calc R . . H12B H 0.6013 0.1706 -0.1207 0.186 Uiso 1 1 calc R . . C13 C 0.5819(10) 0.0682(12) -0.1701(12) 0.187(10) Uani 1 1 d D . . H13A H 0.5598 0.0528 -0.2129 0.224 Uiso 1 1 calc R . . H13B H 0.5504 0.0425 -0.1363 0.224 Uiso 1 1 calc R . . C14 C 0.6686(11) 0.0403(14) -0.1641(12) 0.180(9) Uani 1 1 d D . . H14A H 0.7021 0.0760 -0.1895 0.217 Uiso 1 1 calc R . . H14B H 0.6860 0.0438 -0.1182 0.217 Uiso 1 1 calc R . . C15 C 0.6805(13) -0.0403(15) -0.1870(14) 0.222(12) Uani 1 1 d D . . H15A H 0.6891 -0.0749 -0.1497 0.334 Uiso 1 1 calc R . . H15B H 0.7265 -0.0421 -0.2149 0.334 Uiso 1 1 calc R . . H15C H 0.6338 -0.0575 -0.2116 0.334 Uiso 1 1 calc RD . . C16 C 0.4333(10) 0.1542(12) -0.2192(8) 0.154(6) Uani 1 1 d DU . . H16A H 0.4300 0.0966 -0.2156 0.185 Uiso 1 1 calc R . . H16B H 0.3802 0.1756 -0.2114 0.185 Uiso 1 1 calc R . . C17 C 0.4561(14) 0.1745(14) -0.2856(9) 0.205(8) Uani 1 1 d DU . . H17A H 0.5115 0.1596 -0.2931 0.246 Uiso 1 1 calc R . . H17B H 0.4502 0.2313 -0.2933 0.246 Uiso 1 1 calc R . . C18 C 0.3987(14) 0.1266(17) -0.3318(9) 0.235(10) Uani 1 1 d DU . . H18A H 0.3913 0.0729 -0.3151 0.282 Uiso 1 1 calc R . . H18B H 0.3466 0.1525 -0.3350 0.282 Uiso 1 1 calc R . . C19 C 0.4363(12) 0.1249(11) -0.3952(9) 0.234 Uani 1 1 d DU . . H19A H 0.4908 0.1069 -0.3900 0.351 Uiso 1 1 calc RD . . H19B H 0.4359 0.1776 -0.4140 0.351 Uiso 1 1 calc R . . H19C H 0.4075 0.0891 -0.4241 0.351 Uiso 1 1 calc R . . C20 C 0.5026(11) 0.2746(10) -0.1589(8) 0.171 Uani 1 1 d D . . H20A H 0.5217 0.2873 -0.1146 0.205 Uiso 1 1 calc R . . H20B H 0.5429 0.2920 -0.1898 0.205 Uiso 1 1 calc R . . C21 C 0.4264(11) 0.3178(11) -0.1727(8) 0.171 Uani 1 1 d D . . H21A H 0.3841 0.2948 -0.1465 0.205 Uiso 1 1 calc R . . H21B H 0.4115 0.3113 -0.2190 0.205 Uiso 1 1 calc R . . C22 C 0.4342(12) 0.4088(11) -0.1565(7) 0.171 Uani 1 1 d D . . H22A H 0.4781 0.4309 -0.1814 0.205 Uiso 1 1 calc R . . H22B H 0.3853 0.4357 -0.1708 0.205 Uiso 1 1 calc R . . C23 C 0.4481(8) 0.4246(9) -0.0877(6) 0.171 Uani 1 1 d D . . H23A H 0.4539 0.4810 -0.0810 0.257 Uiso 1 1 calc R . . H23B H 0.4963 0.3979 -0.0731 0.257 Uiso 1 1 calc R . . H23C H 0.4035 0.4054 -0.0629 0.257 Uiso 1 1 calc R . . C24 C 0.9674(7) 0.4315(7) 0.3906(5) 0.083(3) Uani 1 1 d D . . H24A H 0.9871 0.4109 0.4326 0.100 Uiso 1 1 calc R . . H24B H 1.0064 0.4701 0.3755 0.100 Uiso 1 1 calc R . . C25 C 0.8918(7) 0.4742(7) 0.4025(6) 0.092(4) Uani 1 1 d D . . H25A H 0.8504 0.4363 0.4142 0.111 Uiso 1 1 calc R . . H25B H 0.8745 0.5016 0.3625 0.111 Uiso 1 1 calc R . . C26 C 0.9037(9) 0.5345(8) 0.4582(6) 0.107(4) Uani 1 1 d D . . H26A H 0.9064 0.5057 0.4998 0.128 Uiso 1 1 calc R . . H26B H 0.9550 0.5607 0.4526 0.128 Uiso 1 1 calc R . . C27 C 0.8427(11) 0.5945(9) 0.4628(7) 0.154(8) Uani 1 1 d D . . H27A H 0.8653 0.6419 0.4822 0.231 Uiso 1 1 calc R . . H27B H 0.8000 0.5753 0.4897 0.231 Uiso 1 1 calc R . . H27C H 0.8219 0.6066 0.4194 0.231 Uiso 1 1 calc R . . C28 C 0.9176(7) 0.2922(7) 0.3685(5) 0.083(3) Uani 1 1 d D . . H28A H 0.8631 0.3099 0.3762 0.100 Uiso 1 1 calc R . . H28B H 0.9149 0.2511 0.3348 0.100 Uiso 1 1 calc R . . C29 C 0.9500(8) 0.2559(8) 0.4305(6) 0.098(4) Uani 1 1 d D . . H29A H 0.9484 0.2951 0.4657 0.117 Uiso 1 1 calc R . . H29B H 1.0056 0.2410 0.4244 0.117 Uiso 1 1 calc R . . C30 C 0.9031(9) 0.1832(8) 0.4507(7) 0.115(5) Uani 1 1 d D . . H30A H 0.8473 0.1981 0.4558 0.138 Uiso 1 1 calc R . . H30B H 0.9054 0.1439 0.4156 0.138 Uiso 1 1 calc R . . C31 C 0.9322(11) 0.1464(10) 0.5122(7) 0.144(6) Uani 1 1 d D . . H31A H 0.9848 0.1247 0.5058 0.216 Uiso 1 1 calc R . . H31B H 0.8963 0.1044 0.5246 0.216 Uiso 1 1 calc R . . H31C H 0.9346 0.1859 0.5465 0.216 Uiso 1 1 calc R . . C32 C 1.0525(7) 0.3388(8) 0.3289(6) 0.092(4) Uani 1 1 d D . . H32A H 1.0809 0.3853 0.3131 0.110 Uiso 1 1 calc R . . H32B H 1.0772 0.3233 0.3707 0.110 Uiso 1 1 calc R . . C33 C 1.0636(8) 0.2724(9) 0.2807(8) 0.117(5) Uani 1 1 d D . . H33A H 1.0363 0.2850 0.2392 0.140 Uiso 1 1 calc R . . H33B H 1.0410 0.2234 0.2979 0.140 Uiso 1 1 calc R . . C34 C 1.1536(10) 0.2621(13) 0.2697(11) 0.178(9) Uani 1 1 d D . . H34A H 1.1756 0.3139 0.2588 0.214 Uiso 1 1 calc R . . H34B H 1.1782 0.2456 0.3113 0.214 Uiso 1 1 calc R . . C35 C 1.1772(14) 0.2078(16) 0.2209(12) 0.247(14) Uani 1 1 d D . . H35A H 1.1477 0.1589 0.2255 0.371 Uiso 1 1 calc R . . H35B H 1.2336 0.1972 0.2258 0.371 Uiso 1 1 calc R . . H35C H 1.1664 0.2302 0.1780 0.371 Uiso 1 1 calc R . . C36 C 0.9241(7) 0.3892(7) 0.2768(5) 0.082(3) Uani 1 1 d D . . H36A H 0.9205 0.3436 0.2474 0.099 Uiso 1 1 calc R . . H36B H 0.8698 0.4058 0.2864 0.099 Uiso 1 1 calc R . . C37 C 0.9649(8) 0.4553(8) 0.2416(6) 0.102(4) Uani 1 1 d D . . H37A H 1.0195 0.4396 0.2320 0.123 Uiso 1 1 calc R . . H37B H 0.9673 0.5020 0.2700 0.123 Uiso 1 1 calc R . . C38 C 0.9209(10) 0.4764(10) 0.1778(7) 0.142(7) Uani 1 1 d D . . H38A H 0.9137 0.4284 0.1515 0.170 Uiso 1 1 calc R . . H38B H 0.8681 0.4970 0.1879 0.170 Uiso 1 1 calc R . . C39 C 0.9646(12) 0.5361(10) 0.1390(8) 0.155(7) Uani 1 1 d D . . H39A H 1.0092 0.5110 0.1180 0.233 Uiso 1 1 calc R . . H39B H 0.9839 0.5777 0.1678 0.233 Uiso 1 1 calc R . . H39C H 0.9292 0.5585 0.1060 0.233 Uiso 1 1 calc R . . N1 N 0.2462(9) 0.5788(11) 0.1474(6) 0.162(6) Uani 1 1 d . . . N3 N 0.4910(7) 0.1853(8) -0.1651(7) 0.139(4) Uani 1 1 d DU . . N4 N 0.9652(5) 0.3626(6) 0.3414(4) 0.079(2) Uani 1 1 d . . . O1 O 0.1342(5) 0.6103(6) 0.2513(4) 0.108(3) Uani 1 1 d . . . O2 O 0.2493(5) 0.7173(7) 0.2315(4) 0.126(4) Uani 1 1 d . . . O3 O 0.2485(5) 0.4979(6) 0.2687(5) 0.106(3) Uani 1 1 d . . . O4 O 0.3631(5) 0.6061(7) 0.2468(5) 0.122(3) Uani 1 1 d . . . O5 O 0.3655(4) 0.5186(5) 0.3545(4) 0.088(2) Uani 1 1 d . . . O6 O 0.2513(6) 0.3977(5) 0.3775(5) 0.116(3) Uani 1 1 d . . . O7 O 0.2596(4) 0.5447(4) 0.4459(4) 0.082(2) Uani 1 1 d . . . O8 O 0.1401(4) 0.5249(5) 0.3595(4) 0.085(2) Uani 1 1 d . . . O9 O 0.0142(4) 0.6381(6) 0.3440(5) 0.111(3) Uani 1 1 d . . . O10 O 0.1427(4) 0.7437(5) 0.3231(4) 0.089(2) Uani 1 1 d . . . O11 O 0.1480(4) 0.6552(5) 0.4309(4) 0.081(2) Uani 1 1 d . . . O12 O 0.4949(5) 0.6258(6) 0.3332(6) 0.133(4) Uani 1 1 d . . . O13 O 0.3714(4) 0.6519(5) 0.4248(4) 0.095(3) Uani 1 1 d . . . O14 O 0.3678(5) 0.7389(5) 0.3182(5) 0.113(3) Uani 1 1 d . . . O15 O 0.2661(6) 0.6756(6) 0.5323(5) 0.123(3) Uani 1 1 d . . . O16 O 0.2608(5) 0.7624(5) 0.4103(5) 0.098(3) Uani 1 1 d . . . O17 O 0.2574(6) 0.8654(6) 0.3027(7) 0.146(4) Uani 1 1 d . . . O18 O 0.2538(4) 0.6313(4) 0.3362(3) 0.0660(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.1124(10) 0.1554(13) 0.0715(7) 0.0068(8) 0.0130(7) 0.0283(9) Mo2 0.0679(6) 0.0726(6) 0.1062(8) 0.0033(6) 0.0020(5) -0.0009(5) Mo3 0.0504(5) 0.0937(7) 0.0935(7) 0.0167(6) 0.0024(5) 0.0010(5) Mo4 0.0516(5) 0.1003(8) 0.1356(11) 0.0248(7) 0.0159(6) 0.0029(5) Mo5 0.0806(7) 0.0866(7) 0.0779(7) 0.0026(5) -0.0060(5) 0.0046(5) Mo6 0.0714(6) 0.0841(7) 0.1336(10) 0.0430(7) 0.0160(6) 0.0036(5) C1 0.178 0.234 0.135 -0.088 -0.060 0.097 C2 0.178 0.234 0.135 -0.088 -0.060 0.097 C3 0.178 0.234 0.135 -0.088 -0.060 0.097 C4 0.178 0.234 0.135 -0.088 -0.060 0.097 C5 0.178 0.234 0.135 -0.088 -0.060 0.097 C6 0.178 0.234 0.135 -0.088 -0.060 0.097 C7 0.178 0.234 0.135 -0.088 -0.060 0.097 N2 0.178 0.234 0.135 -0.088 -0.060 0.097 O19 0.178 0.234 0.135 -0.088 -0.060 0.097 O20 0.178 0.234 0.135 -0.088 -0.060 0.097 C8 0.172(15) 0.155(14) 0.168(8) 0.044(13) -0.009(11) -0.074(12) C9 0.265(13) 0.216(18) 0.182(9) 0.073(14) -0.062(10) -0.100(15) C10 0.265 0.236 0.171 0.063 -0.065 -0.094 C11 0.265 0.236 0.171 0.063 -0.065 -0.094 C12 0.111(14) 0.19(2) 0.168(18) 0.048(16) 0.012(12) -0.036(14) C13 0.102(14) 0.20(2) 0.25(3) 0.07(2) -0.026(15) -0.017(15) C14 0.127(17) 0.24(3) 0.17(2) -0.01(2) -0.009(15) -0.013(19) C15 0.140(19) 0.28(4) 0.25(3) -0.01(3) 0.022(19) 0.00(2) C16 0.117(12) 0.166(15) 0.179(11) 0.054(12) 0.007(10) -0.019(11) C17 0.185(18) 0.24(2) 0.193(9) 0.066(12) 0.020(13) -0.048(16) C18 0.22(2) 0.31(3) 0.176(11) 0.064(16) -0.002(11) -0.064(19) C19 0.192 0.323 0.185 0.059 -0.021 -0.072 C20 0.184 0.247 0.081 -0.013 -0.003 0.074 C21 0.184 0.247 0.081 -0.013 -0.003 0.074 C22 0.184 0.247 0.081 -0.013 -0.003 0.074 C23 0.184 0.247 0.081 -0.013 -0.003 0.074 C24 0.094(8) 0.089(8) 0.067(7) -0.014(6) -0.004(6) -0.029(7) C25 0.100(9) 0.095(9) 0.082(8) -0.016(7) 0.003(7) -0.009(7) C26 0.133(12) 0.104(11) 0.083(9) -0.024(8) 0.011(8) -0.010(9) C27 0.26(2) 0.106(12) 0.094(11) -0.005(10) 0.019(13) 0.000(15) C28 0.086(8) 0.076(7) 0.087(8) -0.009(6) 0.006(6) -0.024(6) C29 0.099(9) 0.102(10) 0.092(9) 0.005(8) 0.006(7) -0.013(8) C30 0.135(13) 0.090(10) 0.120(12) 0.006(9) 0.021(10) -0.002(9) C31 0.188(18) 0.123(13) 0.120(13) 0.036(11) 0.005(12) 0.005(12) C32 0.082(8) 0.104(10) 0.089(8) 0.000(7) 0.004(7) -0.010(7) C33 0.100(11) 0.120(12) 0.131(13) -0.023(10) 0.013(9) 0.006(9) C34 0.157(18) 0.161(19) 0.22(2) -0.070(17) 0.020(16) 0.024(15) C35 0.21(3) 0.25(3) 0.29(3) -0.12(3) 0.02(2) 0.00(2) C36 0.094(8) 0.086(8) 0.067(7) -0.013(6) -0.007(6) -0.015(7) C37 0.122(11) 0.092(9) 0.093(9) 0.000(8) 0.000(8) -0.021(8) C38 0.188(18) 0.141(15) 0.095(11) 0.026(10) -0.008(11) -0.053(13) C39 0.22(2) 0.130(15) 0.116(13) 0.027(11) -0.013(13) -0.031(14) N1 0.168(13) 0.236(18) 0.081(8) -0.026(10) -0.002(8) 0.055(13) N3 0.102(9) 0.108(9) 0.208(9) 0.001(9) 0.040(8) -0.031(7) N4 0.078(6) 0.085(6) 0.074(6) -0.011(5) -0.001(5) -0.017(5) O1 0.093(6) 0.149(8) 0.082(6) 0.001(6) -0.018(5) 0.007(6) O2 0.072(5) 0.207(11) 0.101(7) 0.081(7) 0.025(5) 0.031(6) O3 0.093(6) 0.106(7) 0.118(7) -0.017(6) -0.003(5) 0.009(5) O4 0.088(6) 0.159(9) 0.119(7) 0.026(7) 0.048(5) 0.030(6) O5 0.061(4) 0.085(5) 0.118(6) 0.002(5) 0.006(4) 0.014(4) O6 0.118(7) 0.072(5) 0.157(9) 0.003(6) 0.006(6) -0.007(5) O7 0.077(5) 0.077(5) 0.092(5) 0.025(4) 0.001(4) 0.005(4) O8 0.059(4) 0.087(5) 0.111(6) 0.005(5) 0.002(4) -0.013(4) O9 0.053(4) 0.137(8) 0.143(8) 0.024(6) -0.001(5) 0.009(5) O10 0.066(4) 0.094(6) 0.106(6) 0.025(5) 0.005(4) 0.020(4) O11 0.066(4) 0.087(5) 0.091(5) 0.011(4) 0.019(4) 0.011(4) O12 0.053(5) 0.131(8) 0.216(11) 0.037(8) 0.022(6) 0.005(5) O13 0.065(5) 0.085(5) 0.133(7) 0.006(5) -0.024(5) -0.007(4) O14 0.064(5) 0.107(7) 0.168(9) 0.044(6) 0.020(5) -0.014(5) O15 0.132(8) 0.124(8) 0.113(7) -0.014(6) -0.012(6) 0.020(6) O16 0.088(6) 0.076(5) 0.130(7) -0.010(5) -0.003(5) 0.001(4) O17 0.110(8) 0.102(7) 0.227(13) 0.061(8) 0.025(8) 0.001(6) O18 0.049(3) 0.078(4) 0.071(4) 0.014(3) 0.007(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.714(12) . ? Mo1 O2 1.857(12) . ? Mo1 O4 1.943(9) . ? Mo1 O1 1.956(9) . ? Mo1 O3 1.991(10) . ? Mo1 O18 2.210(7) . ? Mo2 O6 1.675(9) . ? Mo2 O3 1.841(9) . ? Mo2 O8 1.906(7) . ? Mo2 O7 1.938(8) . ? Mo2 O5 1.957(7) . ? Mo2 O18 2.330(7) . ? Mo3 O9 1.681(7) . ? Mo3 O10 1.889(8) . ? Mo3 O1 1.900(9) . ? Mo3 O11 1.919(8) . ? Mo3 O8 1.955(8) . ? Mo3 O18 2.318(6) . ? Mo4 O12 1.693(8) . ? Mo4 O4 1.890(10) . ? Mo4 O13 1.896(9) . ? Mo4 O5 1.908(8) . ? Mo4 O14 1.960(9) . ? Mo4 O18 2.326(6) . ? Mo5 O15 1.673(10) . ? Mo5 O7 1.871(8) . ? Mo5 O11 1.918(7) . ? Mo5 O13 1.928(8) . ? Mo5 O16 1.964(9) . ? Mo5 O18 2.368(7) . ? Mo6 O17 1.670(10) . ? Mo6 O16 1.872(9) . ? Mo6 O14 1.893(8) . ? Mo6 O2 1.944(11) . ? Mo6 O10 1.962(7) . ? Mo6 O18 2.313(7) . ? C1 C2 1.375(14) . ? C1 C6 1.399(14) . ? C1 N1 1.475(19) . ? C2 C3 1.348(13) . ? C2 C7 1.50(2) . ? C3 C4 1.381(14) . ? C3 H3 0.9300 . ? C4 C5 1.374(13) . ? C4 N2 1.417(9) . ? C5 C6 1.352(13) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? N2 O20 1.295(8) . ? N2 O19 1.301(8) . ? C8 C9 1.474(14) . ? C8 N3 1.508(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.554(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.497(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.471(14) . ? C12 N3 1.513(13) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.520(14) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.443(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.445(14) . ? C16 N3 1.534(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.549(15) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.440(15) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.483(13) . ? C20 N3 1.513(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.565(14) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.433(13) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.471(12) . ? C24 N4 1.525(13) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.524(12) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.434(13) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.488(12) . ? C28 N4 1.529(13) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.507(12) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.464(13) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.493(12) . ? C32 N4 1.533(14) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.529(13) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.405(14) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.488(12) . ? C36 N4 1.530(13) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.515(13) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.472(13) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 O2 107.3(7) . . ? N1 Mo1 O4 100.3(6) . . ? O2 Mo1 O4 89.3(4) . . ? N1 Mo1 O1 103.3(6) . . ? O2 Mo1 O1 88.4(4) . . ? O4 Mo1 O1 155.9(4) . . ? N1 Mo1 O3 98.1(7) . . ? O2 Mo1 O3 154.6(4) . . ? O4 Mo1 O3 85.7(4) . . ? O1 Mo1 O3 86.2(4) . . ? N1 Mo1 O18 174.9(6) . . ? O2 Mo1 O18 77.6(3) . . ? O4 Mo1 O18 78.0(3) . . ? O1 Mo1 O18 78.0(3) . . ? O3 Mo1 O18 77.0(3) . . ? O6 Mo2 O3 103.8(5) . . ? O6 Mo2 O8 104.9(4) . . ? O3 Mo2 O8 89.5(4) . . ? O6 Mo2 O7 102.8(4) . . ? O3 Mo2 O7 153.1(4) . . ? O8 Mo2 O7 87.1(3) . . ? O6 Mo2 O5 101.8(4) . . ? O3 Mo2 O5 86.7(4) . . ? O8 Mo2 O5 153.2(3) . . ? O7 Mo2 O5 84.4(3) . . ? O6 Mo2 O18 178.2(4) . . ? O3 Mo2 O18 76.9(3) . . ? O8 Mo2 O18 76.7(3) . . ? O7 Mo2 O18 76.3(3) . . ? O5 Mo2 O18 76.6(3) . . ? O9 Mo3 O10 104.0(4) . . ? O9 Mo3 O1 103.0(4) . . ? O10 Mo3 O1 89.6(4) . . ? O9 Mo3 O11 103.4(4) . . ? O10 Mo3 O11 87.7(3) . . ? O1 Mo3 O11 153.3(3) . . ? O9 Mo3 O8 102.5(4) . . ? O10 Mo3 O8 153.4(3) . . ? O1 Mo3 O8 85.5(4) . . ? O11 Mo3 O8 85.1(3) . . ? O9 Mo3 O18 178.6(4) . . ? O10 Mo3 O18 77.3(3) . . ? O1 Mo3 O18 76.4(3) . . ? O11 Mo3 O18 77.1(3) . . ? O8 Mo3 O18 76.1(3) . . ? O12 Mo4 O4 102.7(5) . . ? O12 Mo4 O13 103.8(5) . . ? O4 Mo4 O13 153.3(3) . . ? O12 Mo4 O5 104.2(4) . . ? O4 Mo4 O5 87.5(4) . . ? O13 Mo4 O5 88.3(4) . . ? O12 Mo4 O14 102.5(4) . . ? O4 Mo4 O14 87.1(4) . . ? O13 Mo4 O14 85.0(4) . . ? O5 Mo4 O14 153.3(3) . . ? O12 Mo4 O18 177.9(4) . . ? O4 Mo4 O18 76.2(3) . . ? O13 Mo4 O18 77.2(3) . . ? O5 Mo4 O18 77.6(3) . . ? O14 Mo4 O18 75.8(3) . . ? O15 Mo5 O7 104.5(4) . . ? O15 Mo5 O11 104.2(4) . . ? O7 Mo5 O11 88.2(3) . . ? O15 Mo5 O13 104.3(4) . . ? O7 Mo5 O13 87.5(3) . . ? O11 Mo5 O13 151.4(3) . . ? O15 Mo5 O16 103.7(5) . . ? O7 Mo5 O16 151.8(4) . . ? O11 Mo5 O16 85.6(3) . . ? O13 Mo5 O16 84.8(3) . . ? O15 Mo5 O18 178.9(4) . . ? O7 Mo5 O18 76.6(3) . . ? O11 Mo5 O18 75.9(3) . . ? O13 Mo5 O18 75.6(3) . . ? O16 Mo5 O18 75.2(3) . . ? O17 Mo6 O16 103.3(5) . . ? O17 Mo6 O14 104.5(4) . . ? O16 Mo6 O14 88.7(4) . . ? O17 Mo6 O2 105.0(6) . . ? O16 Mo6 O2 151.6(4) . . ? O14 Mo6 O2 87.0(4) . . ? O17 Mo6 O10 102.0(4) . . ? O16 Mo6 O10 86.9(3) . . ? O14 Mo6 O10 153.4(4) . . ? O2 Mo6 O10 84.5(4) . . ? O17 Mo6 O18 177.6(5) . . ? O16 Mo6 O18 78.2(3) . . ? O14 Mo6 O18 77.3(3) . . ? O2 Mo6 O18 73.4(3) . . ? O10 Mo6 O18 76.1(3) . . ? C2 C1 C6 115.8(13) . . ? C2 C1 N1 115.7(16) . . ? C6 C1 N1 128.2(16) . . ? C3 C2 C1 125.8(15) . . ? C3 C2 C7 119.8(17) . . ? C1 C2 C7 111.6(14) . . ? C2 C3 C4 114.2(13) . . ? C2 C3 H3 122.9 . . ? C4 C3 H3 122.9 . . ? C5 C4 C3 122.9(12) . . ? C5 C4 N2 115.1(12) . . ? C3 C4 N2 119.8(12) . . ? C6 C5 C4 119.2(14) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C1 120.6(14) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O20 N2 O19 115.3(9) . . ? O20 N2 C4 115.8(11) . . ? O19 N2 C4 115.3(11) . . ? C9 C8 N3 118.8(14) . . ? C9 C8 H8A 107.6 . . ? N3 C8 H8A 107.6 . . ? C9 C8 H8B 107.6 . . ? N3 C8 H8B 107.6 . . ? H8A C8 H8B 107.1 . . ? C8 C9 C10 112.8(14) . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 112.5(15) . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N3 112.6(14) . . ? C13 C12 H12A 109.1 . . ? N3 C12 H12A 109.1 . . ? C13 C12 H12B 109.1 . . ? N3 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 110.8(15) . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C13 113.5(17) . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N3 114.3(14) . . ? C17 C16 H16A 108.7 . . ? N3 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? N3 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C16 C17 C18 105.7(14) . . ? C16 C17 H17A 110.6 . . ? C18 C17 H17A 110.6 . . ? C16 C17 H17B 110.6 . . ? C18 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? C19 C18 C17 105.9(15) . . ? C19 C18 H18A 110.6 . . ? C17 C18 H18A 110.6 . . ? C19 C18 H18B 110.6 . . ? C17 C18 H18B 110.6 . . ? H18A C18 H18B 108.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N3 111.1(15) . . ? C21 C20 H20A 109.4 . . ? N3 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? N3 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C20 C21 C22 111.6(14) . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C23 C22 C21 113.3(13) . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N4 117.7(9) . . ? C25 C24 H24A 107.9 . . ? N4 C24 H24A 107.9 . . ? C25 C24 H24B 107.9 . . ? N4 C24 H24B 107.9 . . ? H24A C24 H24B 107.2 . . ? C24 C25 C26 110.1(10) . . ? C24 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? C24 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.2 . . ? C27 C26 C25 115.5(12) . . ? C27 C26 H26A 108.4 . . ? C25 C26 H26A 108.4 . . ? C27 C26 H26B 108.4 . . ? C25 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N4 115.9(9) . . ? C29 C28 H28A 108.3 . . ? N4 C28 H28A 108.3 . . ? C29 C28 H28B 108.3 . . ? N4 C28 H28B 108.3 . . ? H28A C28 H28B 107.4 . . ? C28 C29 C30 112.2(10) . . ? C28 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? C28 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 C29 113.9(12) . . ? C31 C30 H30A 108.8 . . ? C29 C30 H30A 108.8 . . ? C31 C30 H30B 108.8 . . ? C29 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 N4 115.5(10) . . ? C33 C32 H32A 108.4 . . ? N4 C32 H32A 108.4 . . ? C33 C32 H32B 108.4 . . ? N4 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? C32 C33 C34 108.2(11) . . ? C32 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? C32 C33 H33B 110.1 . . ? C34 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? C35 C34 C33 117.6(16) . . ? C35 C34 H34A 107.9 . . ? C33 C34 H34A 107.9 . . ? C35 C34 H34B 107.9 . . ? C33 C34 H34B 107.9 . . ? H34A C34 H34B 107.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 N4 115.2(9) . . ? C37 C36 H36A 108.5 . . ? N4 C36 H36A 108.5 . . ? C37 C36 H36B 108.5 . . ? N4 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C36 C37 C38 111.4(10) . . ? C36 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? C36 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? C39 C38 C37 112.2(12) . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38B 109.2 . . ? C37 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C1 N1 Mo1 152.5(15) . . ? C8 N3 C20 106.6(14) . . ? C8 N3 C12 111.4(14) . . ? C20 N3 C12 101.9(12) . . ? C8 N3 C16 99.0(11) . . ? C20 N3 C16 118.2(14) . . ? C12 N3 C16 119.3(14) . . ? C24 N4 C28 110.9(8) . . ? C24 N4 C36 110.1(9) . . ? C28 N4 C36 107.8(8) . . ? C24 N4 C32 107.1(8) . . ? C28 N4 C32 110.9(9) . . ? C36 N4 C32 110.2(9) . . ? Mo3 O1 Mo1 114.2(4) . . ? Mo1 O2 Mo6 117.3(4) . . ? Mo2 O3 Mo1 115.2(5) . . ? Mo4 O4 Mo1 114.9(4) . . ? Mo4 O5 Mo2 116.2(4) . . ? Mo5 O7 Mo2 118.6(4) . . ? Mo2 O8 Mo3 117.0(4) . . ? Mo3 O10 Mo6 116.5(4) . . ? Mo5 O11 Mo3 117.9(3) . . ? Mo4 O13 Mo5 118.3(4) . . ? Mo6 O14 Mo4 116.8(4) . . ? Mo6 O16 Mo5 117.6(4) . . ? Mo1 O18 Mo6 91.7(2) . . ? Mo1 O18 Mo3 91.3(2) . . ? Mo6 O18 Mo3 90.0(2) . . ? Mo1 O18 Mo4 90.9(2) . . ? Mo6 O18 Mo4 90.1(2) . . ? Mo3 O18 Mo4 177.9(3) . . ? Mo1 O18 Mo2 90.9(3) . . ? Mo6 O18 Mo2 177.4(3) . . ? Mo3 O18 Mo2 90.2(2) . . ? Mo4 O18 Mo2 89.6(2) . . ? Mo1 O18 Mo5 179.2(4) . . ? Mo6 O18 Mo5 89.0(2) . . ? Mo3 O18 Mo5 89.1(2) . . ? Mo4 O18 Mo5 88.7(2) . . ? Mo2 O18 Mo5 88.4(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.557 _refine_diff_density_min -2.186 _refine_diff_density_rms 0.142 # Attachment 'MePhNO2.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 671420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H78 Mo6 N4 O20' _chemical_formula_weight 1498.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4519(7) _cell_length_b 19.5005(11) _cell_length_c 23.6287(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.0620(10) _cell_angle_gamma 90.00 _cell_volume 5733.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 9708 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 1.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6891 _exptl_absorpt_correction_T_max 0.7752 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43975 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11249 _reflns_number_gt 8650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+3.6860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11249 _refine_ls_number_parameters 659 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.02389(2) 0.675742(15) 0.430570(13) 0.05137(9) Uani 1 1 d . . . Mo2 Mo 0.02158(3) 0.841476(16) 0.430051(13) 0.05570(10) Uani 1 1 d . . . Mo3 Mo -0.19970(3) 0.754468(14) 0.453889(13) 0.05045(9) Uani 1 1 d . . . Mo4 Mo 0.04930(3) 0.755548(17) 0.311694(14) 0.05646(10) Uani 1 1 d . . . Mo5 Mo -0.16993(2) 0.668087(15) 0.336210(13) 0.05041(9) Uani 1 1 d . . . Mo6 Mo -0.17699(3) 0.837057(16) 0.333806(14) 0.05782(10) Uani 1 1 d . . . C1 C 0.1613(3) 0.58439(19) 0.51216(15) 0.0578(9) Uani 1 1 d . . . C2 C 0.1769(3) 0.5141(2) 0.50788(19) 0.0733(12) Uani 1 1 d . . . C3 C 0.2368(4) 0.4824(3) 0.5506(3) 0.115(2) Uani 1 1 d . . . H3 H 0.2476 0.4353 0.5491 0.137 Uiso 1 1 calc R . . C4 C 0.2809(5) 0.5187(5) 0.5953(3) 0.140(3) Uani 1 1 d . A . H4 H 0.3224 0.4967 0.6233 0.167 Uiso 1 1 calc R . . C5 C 0.2630(4) 0.5881(4) 0.5982(2) 0.107(2) Uani 1 1 d D . . C6 C 0.2047(3) 0.6215(3) 0.55732(18) 0.0786(12) Uani 1 1 d . A . H6 H 0.1941 0.6686 0.5596 0.094 Uiso 1 1 calc R . . C7 C 0.1270(5) 0.4756(2) 0.4592(2) 0.1116(19) Uani 1 1 d . . . H7A H 0.1447 0.4279 0.4627 0.167 Uiso 1 1 calc R . . H7B H 0.1538 0.4931 0.4244 0.167 Uiso 1 1 calc R . . H7C H 0.0504 0.4811 0.4590 0.167 Uiso 1 1 calc R . . C8 C 0.4795(4) 0.7152(4) 0.3973(2) 0.1076(18) Uani 1 1 d . . . H8A H 0.5295 0.7527 0.4040 0.129 Uiso 1 1 calc R . . H8B H 0.5199 0.6727 0.4006 0.129 Uiso 1 1 calc R . . C9 C 0.3959(5) 0.7165(4) 0.4434(2) 0.144(3) Uani 1 1 d . . . H9A H 0.3601 0.7607 0.4431 0.173 Uiso 1 1 calc R . . H9B H 0.3422 0.6815 0.4357 0.173 Uiso 1 1 calc R . . C10 C 0.4493(6) 0.7041(6) 0.5015(3) 0.176(4) Uani 1 1 d . . . H10A H 0.3961 0.7101 0.5300 0.211 Uiso 1 1 calc R . . H10B H 0.5047 0.7384 0.5081 0.211 Uiso 1 1 calc R . . C11 C 0.5011(8) 0.6311(6) 0.5089(4) 0.216(5) Uani 1 1 d . . . H11A H 0.4480 0.5966 0.5002 0.323 Uiso 1 1 calc R . . H11B H 0.5275 0.6255 0.5473 0.323 Uiso 1 1 calc R . . H11C H 0.5595 0.6265 0.4837 0.323 Uiso 1 1 calc R . . C12 C 0.3524(3) 0.6629(3) 0.3250(2) 0.0984(17) Uani 1 1 d . . . H12A H 0.2920 0.6689 0.3493 0.118 Uiso 1 1 calc R . . H12B H 0.3254 0.6672 0.2861 0.118 Uiso 1 1 calc R . . C13 C 0.3963(4) 0.5908(4) 0.3335(3) 0.117(2) Uani 1 1 d . . . H13A H 0.4545 0.5833 0.3080 0.140 Uiso 1 1 calc R . . H13B H 0.4252 0.5861 0.3720 0.140 Uiso 1 1 calc R . . C14 C 0.3109(6) 0.5375(4) 0.3227(3) 0.151(3) Uani 1 1 d . . . H14A H 0.2513 0.5467 0.3469 0.181 Uiso 1 1 calc R . . H14B H 0.2844 0.5412 0.2837 0.181 Uiso 1 1 calc R . . C15 C 0.3489(7) 0.4668(5) 0.3331(4) 0.182(3) Uani 1 1 d . . . H15A H 0.4114 0.4584 0.3115 0.272 Uiso 1 1 calc R . . H15B H 0.2933 0.4350 0.3218 0.272 Uiso 1 1 calc R . . H15C H 0.3667 0.4610 0.3726 0.272 Uiso 1 1 calc R . . C16 C 0.5260(3) 0.7157(3) 0.29806(18) 0.0852(13) Uani 1 1 d . . . H16A H 0.5623 0.6724 0.3050 0.102 Uiso 1 1 calc R . . H16B H 0.5767 0.7521 0.3075 0.102 Uiso 1 1 calc R . . C17 C 0.4951(4) 0.7205(4) 0.2355(2) 0.1106(18) Uani 1 1 d . . . H17A H 0.4506 0.6815 0.2248 0.133 Uiso 1 1 calc R . . H17B H 0.4529 0.7617 0.2288 0.133 Uiso 1 1 calc R . . C18 C 0.5897(4) 0.7221(4) 0.1992(2) 0.127(2) Uani 1 1 d . . . H18A H 0.6367 0.7591 0.2120 0.152 Uiso 1 1 calc R . . H18B H 0.6291 0.6795 0.2044 0.152 Uiso 1 1 calc R . . C19 C 0.5647(6) 0.7314(5) 0.1388(3) 0.165(3) Uani 1 1 d . . . H19A H 0.5168 0.6957 0.1258 0.248 Uiso 1 1 calc R . . H19B H 0.6298 0.7293 0.1183 0.248 Uiso 1 1 calc R . . H19C H 0.5311 0.7752 0.1327 0.248 Uiso 1 1 calc R . . C20 C 0.3726(4) 0.7874(3) 0.3286(2) 0.1066(18) Uani 1 1 d . . . H20A H 0.3182 0.7904 0.3569 0.128 Uiso 1 1 calc R . . H20B H 0.3357 0.7863 0.2918 0.128 Uiso 1 1 calc R . . C21 C 0.4419(5) 0.8528(4) 0.3323(3) 0.148(3) Uani 1 1 d . . . H21A H 0.4794 0.8545 0.3690 0.177 Uiso 1 1 calc R . . H21B H 0.4954 0.8511 0.3035 0.177 Uiso 1 1 calc R . . C22 C 0.3767(6) 0.9158(4) 0.3244(4) 0.155(3) Uani 1 1 d . . . H22A H 0.3310 0.9211 0.3566 0.186 Uiso 1 1 calc R . . H22B H 0.3303 0.9106 0.2908 0.186 Uiso 1 1 calc R . . C23 C 0.4430(9) 0.9796(5) 0.3186(4) 0.228(5) Uani 1 1 d . . . H23A H 0.4858 0.9867 0.3527 0.342 Uiso 1 1 calc R . . H23B H 0.3963 1.0182 0.3122 0.342 Uiso 1 1 calc R . . H23C H 0.4891 0.9746 0.2872 0.342 Uiso 1 1 calc R . . C24 C 0.8923(4) 0.5700(2) 0.08826(18) 0.0811(12) Uani 1 1 d . . . H24A H 0.9222 0.5913 0.0552 0.097 Uiso 1 1 calc R . . H24B H 0.9007 0.5209 0.0840 0.097 Uiso 1 1 calc R . . C25 C 0.7754(4) 0.5853(3) 0.0872(2) 0.1089(17) Uani 1 1 d . . . H25A H 0.7643 0.6345 0.0869 0.131 Uiso 1 1 calc R . . H25B H 0.7438 0.5667 0.1208 0.131 Uiso 1 1 calc R . . C26 C 0.7217(5) 0.5535(3) 0.0346(3) 0.144(3) Uani 1 1 d . . . H26A H 0.7617 0.5669 0.0019 0.173 Uiso 1 1 calc R . . H26B H 0.7264 0.5040 0.0379 0.173 Uiso 1 1 calc R . . C27 C 0.6108(7) 0.5719(5) 0.0243(4) 0.217(4) Uani 1 1 d . . . H27A H 0.5711 0.5626 0.0575 0.325 Uiso 1 1 calc R . . H27B H 0.5814 0.5456 -0.0069 0.325 Uiso 1 1 calc R . . H27C H 0.6058 0.6199 0.0154 0.325 Uiso 1 1 calc R . . C28 C 0.9504(4) 0.6684(2) 0.15064(18) 0.0838(13) Uani 1 1 d . . . H28A H 0.8760 0.6786 0.1583 0.101 Uiso 1 1 calc R . . H28B H 0.9926 0.6784 0.1850 0.101 Uiso 1 1 calc R . . C29 C 0.9848(5) 0.7156(2) 0.10612(19) 0.0875(14) Uani 1 1 d . . . H29A H 0.9419 0.7078 0.0716 0.105 Uiso 1 1 calc R . . H29B H 1.0595 0.7069 0.0981 0.105 Uiso 1 1 calc R . . C30 C 0.9716(4) 0.7908(2) 0.1255(2) 0.0866(14) Uani 1 1 d . . . H30A H 1.0167 0.7982 0.1593 0.104 Uiso 1 1 calc R . . H30B H 0.9974 0.8209 0.0962 0.104 Uiso 1 1 calc R . . C31 C 0.8592(5) 0.8109(3) 0.1379(2) 0.1085(17) Uani 1 1 d . . . H31A H 0.8124 0.7998 0.1060 0.163 Uiso 1 1 calc R . . H31B H 0.8562 0.8593 0.1450 0.163 Uiso 1 1 calc R . . H31C H 0.8365 0.7865 0.1707 0.163 Uiso 1 1 calc R . . C32 C 1.0726(4) 0.5727(2) 0.12601(19) 0.0834(13) Uani 1 1 d . . . H32A H 1.0746 0.5236 0.1193 0.100 Uiso 1 1 calc R . . H32B H 1.0905 0.5950 0.0909 0.100 Uiso 1 1 calc R . . C33 C 1.1590(5) 0.5896(4) 0.1695(3) 0.141(2) Uani 1 1 d . . . H33A H 1.1491 0.5631 0.2037 0.169 Uiso 1 1 calc R . . H33B H 1.1564 0.6379 0.1791 0.169 Uiso 1 1 calc R . . C34 C 1.2684(6) 0.5719(6) 0.1442(5) 0.199(4) Uani 1 1 d . . . H34A H 1.3233 0.5757 0.1742 0.239 Uiso 1 1 calc R . . H34B H 1.2661 0.5243 0.1323 0.239 Uiso 1 1 calc R . . C35 C 1.3026(7) 0.6127(6) 0.0966(6) 0.253(6) Uani 1 1 d . . . H35A H 1.2507 0.6085 0.0658 0.379 Uiso 1 1 calc R . . H35B H 1.3712 0.5967 0.0849 0.379 Uiso 1 1 calc R . . H35C H 1.3083 0.6599 0.1078 0.379 Uiso 1 1 calc R . . C36 C 0.9231(4) 0.5590(2) 0.19434(18) 0.0868(13) Uani 1 1 d . . . H36A H 0.9702 0.5754 0.2250 0.104 Uiso 1 1 calc R . . H36B H 0.8513 0.5753 0.2015 0.104 Uiso 1 1 calc R . . C37 C 0.9218(5) 0.4842(2) 0.1965(2) 0.0997(16) Uani 1 1 d . . . H37A H 0.9912 0.4666 0.1860 0.120 Uiso 1 1 calc R . . H37B H 0.8678 0.4668 0.1695 0.120 Uiso 1 1 calc R . . C38 C 0.8965(5) 0.4593(3) 0.2570(2) 0.1078(18) Uani 1 1 d . . . H38A H 0.8318 0.4823 0.2685 0.129 Uiso 1 1 calc R . . H38B H 0.8807 0.4106 0.2551 0.129 Uiso 1 1 calc R . . C39 C 0.9799(6) 0.4698(3) 0.3013(2) 0.139(3) Uani 1 1 d . . . H39A H 1.0455 0.4485 0.2903 0.208 Uiso 1 1 calc R . . H39B H 0.9575 0.4498 0.3361 0.208 Uiso 1 1 calc R . . H39C H 0.9917 0.5181 0.3066 0.208 Uiso 1 1 calc R . . N1 N 0.1008(2) 0.61926(15) 0.47191(13) 0.0621(8) Uani 1 1 d . . . N3 N 0.4324(3) 0.7209(3) 0.33704(16) 0.0925(12) Uani 1 1 d . . . N4 N 0.9591(3) 0.59177(16) 0.13880(13) 0.0683(8) Uani 1 1 d . . . O1 O 0.0796(2) 0.76299(12) 0.46351(11) 0.0593(6) Uani 1 1 d . . . O2 O -0.06943(17) 0.61888(12) 0.38524(10) 0.0546(6) Uani 1 1 d . . . O3 O -0.09820(19) 0.69053(12) 0.48055(9) 0.0537(6) Uani 1 1 d . . . O4 O 0.0838(3) 0.90664(15) 0.46435(13) 0.0893(9) Uani 1 1 d . . . O5 O -0.08277(19) 0.89014(12) 0.37998(10) 0.0634(7) Uani 1 1 d . . . O6 O -0.1051(2) 0.82695(12) 0.47578(10) 0.0585(6) Uani 1 1 d . . . O7 O 0.10249(19) 0.82683(13) 0.36483(10) 0.0608(6) Uani 1 1 d . . . O8 O -0.2932(3) 0.75552(14) 0.50339(13) 0.0783(9) Uani 1 1 d . . . O9 O -0.26041(19) 0.81779(12) 0.39711(11) 0.0593(6) Uani 1 1 d . . . O10 O -0.25291(17) 0.68403(12) 0.40077(10) 0.0516(5) Uani 1 1 d . . . O11 O 0.1407(2) 0.75556(16) 0.26074(13) 0.0845(10) Uani 1 1 d . . . O12 O -0.04598(19) 0.68349(13) 0.28926(10) 0.0591(6) Uani 1 1 d . . . O13 O -0.0540(2) 0.82038(14) 0.28659(10) 0.0627(7) Uani 1 1 d . . . O14 O -0.2392(2) 0.60584(14) 0.30116(12) 0.0756(8) Uani 1 1 d . . . O15 O -0.2271(2) 0.74975(11) 0.30374(11) 0.0579(6) Uani 1 1 d . . . O16 O -0.2504(2) 0.89474(16) 0.29655(14) 0.0922(10) Uani 1 1 d . . . O17 O 0.11125(18) 0.69225(13) 0.36757(10) 0.0580(6) Uani 1 1 d . . . O18 O -0.07248(16) 0.75352(9) 0.38392(8) 0.0403(5) Uani 1 1 d . . . N2 N 0.3052(8) 0.6387(4) 0.6433(3) 0.099(3) Uani 0.582(13) 1 d PDU A 1 O19 O 0.2811(6) 0.7052(5) 0.6443(3) 0.127(3) Uani 0.582(13) 1 d PDU A 1 O20 O 0.3611(7) 0.6132(5) 0.6843(3) 0.142(4) Uani 0.582(13) 1 d PDU A 1 N2' N 0.3282(11) 0.6053(8) 0.6460(5) 0.135(5) Uani 0.418(13) 1 d PDU A 2 O19' O 0.3866(10) 0.5624(7) 0.6728(5) 0.162(6) Uani 0.418(13) 1 d PDU A 2 O20' O 0.2995(9) 0.6657(7) 0.6590(5) 0.114(4) Uani 0.418(13) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.04350(17) 0.05355(17) 0.05649(19) 0.01133(13) -0.00628(14) 0.00372(13) Mo2 0.0615(2) 0.05217(17) 0.05281(19) 0.00122(13) -0.00675(15) -0.01512(14) Mo3 0.04954(19) 0.05671(18) 0.04576(18) -0.00153(12) 0.01095(14) -0.00053(12) Mo4 0.04047(18) 0.0855(2) 0.04377(18) 0.00423(14) 0.00593(13) -0.00479(14) Mo5 0.04084(17) 0.05790(18) 0.05221(19) -0.01105(13) -0.00206(13) -0.00246(12) Mo6 0.05181(19) 0.05980(19) 0.0612(2) 0.01784(14) -0.00722(15) 0.00486(14) C1 0.0413(19) 0.068(2) 0.064(2) 0.0205(18) -0.0018(17) 0.0030(16) C2 0.063(2) 0.064(2) 0.094(3) 0.029(2) 0.021(2) 0.0071(19) C3 0.082(4) 0.102(4) 0.161(6) 0.077(4) 0.016(4) 0.021(3) C4 0.068(4) 0.204(8) 0.146(6) 0.110(6) -0.008(4) 0.003(4) C5 0.066(3) 0.192(7) 0.063(3) 0.024(4) -0.008(2) -0.034(4) C6 0.055(2) 0.107(3) 0.074(3) 0.011(3) 0.001(2) -0.010(2) C7 0.134(5) 0.070(3) 0.134(5) -0.010(3) 0.051(4) -0.014(3) C8 0.050(3) 0.200(6) 0.073(3) -0.003(4) 0.003(2) -0.016(3) C9 0.076(4) 0.279(9) 0.078(4) -0.019(5) 0.015(3) -0.018(5) C10 0.101(5) 0.349(13) 0.078(4) -0.023(7) 0.020(4) -0.065(7) C11 0.171(9) 0.343(15) 0.134(7) 0.050(9) 0.019(6) -0.004(9) C12 0.043(2) 0.166(6) 0.087(3) -0.004(3) 0.003(2) -0.004(3) C13 0.075(4) 0.162(6) 0.112(4) 0.006(4) 0.002(3) -0.010(4) C14 0.119(6) 0.178(8) 0.156(6) 0.040(6) 0.002(5) -0.039(6) C15 0.165(8) 0.197(9) 0.183(8) 0.012(7) 0.017(6) -0.055(7) C16 0.040(2) 0.143(4) 0.073(3) 0.002(3) 0.009(2) 0.005(2) C17 0.064(3) 0.186(6) 0.082(4) 0.020(4) 0.005(3) 0.009(3) C18 0.075(4) 0.238(7) 0.067(3) 0.011(4) 0.005(3) 0.017(4) C19 0.098(5) 0.315(11) 0.083(4) 0.011(5) 0.008(4) 0.005(5) C20 0.054(3) 0.156(5) 0.110(4) -0.021(4) 0.003(3) 0.007(3) C21 0.087(4) 0.162(7) 0.195(7) -0.044(6) 0.007(5) 0.002(5) C22 0.131(6) 0.168(8) 0.169(7) -0.035(6) 0.031(5) 0.012(6) C23 0.251(11) 0.154(8) 0.285(12) -0.063(8) 0.084(9) -0.031(8) C24 0.103(4) 0.065(2) 0.074(3) 0.004(2) -0.012(3) -0.011(2) C25 0.095(4) 0.107(4) 0.123(5) 0.023(3) -0.008(3) -0.010(3) C26 0.110(5) 0.131(5) 0.186(7) 0.031(5) -0.053(5) -0.042(4) C27 0.158(8) 0.199(9) 0.286(11) 0.053(8) -0.077(8) -0.064(7) C28 0.119(4) 0.069(3) 0.064(3) -0.002(2) 0.005(3) 0.000(2) C29 0.120(4) 0.078(3) 0.065(3) -0.001(2) 0.006(3) 0.000(3) C30 0.116(4) 0.064(3) 0.079(3) -0.001(2) -0.007(3) -0.010(3) C31 0.123(5) 0.096(4) 0.106(4) -0.011(3) 0.004(3) 0.005(3) C32 0.092(3) 0.077(3) 0.081(3) 0.003(2) -0.003(3) -0.001(2) C33 0.119(5) 0.148(6) 0.152(6) -0.001(5) -0.041(5) 0.011(4) C34 0.091(6) 0.221(11) 0.286(13) 0.021(9) 0.001(7) -0.017(6) C35 0.122(7) 0.290(15) 0.347(17) -0.016(13) 0.016(9) -0.062(8) C36 0.116(4) 0.075(3) 0.071(3) 0.002(2) 0.022(3) 0.006(3) C37 0.137(4) 0.076(3) 0.089(3) 0.001(3) 0.034(3) 0.018(3) C38 0.164(5) 0.075(3) 0.087(4) 0.012(3) 0.042(4) 0.028(3) C39 0.210(8) 0.108(5) 0.098(4) -0.002(3) -0.012(5) 0.045(5) N1 0.0512(17) 0.0615(18) 0.073(2) 0.0179(15) -0.0095(15) 0.0041(14) N3 0.0414(19) 0.162(4) 0.074(2) -0.008(3) 0.0012(17) -0.001(2) N4 0.084(2) 0.0609(19) 0.0597(19) 0.0025(15) 0.0067(17) -0.0004(17) O1 0.0595(16) 0.0646(15) 0.0522(15) 0.0093(11) -0.0190(12) -0.0098(11) O2 0.0481(14) 0.0477(13) 0.0678(16) -0.0043(11) -0.0001(11) 0.0040(10) O3 0.0579(14) 0.0578(13) 0.0454(13) 0.0123(10) 0.0032(11) 0.0006(11) O4 0.107(2) 0.0710(18) 0.088(2) -0.0080(15) -0.0197(18) -0.0339(17) O5 0.0723(17) 0.0467(13) 0.0707(17) 0.0108(11) -0.0041(14) -0.0038(11) O6 0.0731(17) 0.0560(14) 0.0467(13) -0.0074(10) 0.0046(12) -0.0027(12) O7 0.0494(14) 0.0743(16) 0.0584(15) 0.0161(12) -0.0032(11) -0.0193(12) O8 0.077(2) 0.091(2) 0.0680(19) -0.0043(14) 0.0317(16) 0.0021(14) O9 0.0501(14) 0.0603(14) 0.0679(16) 0.0089(12) 0.0081(12) 0.0136(11) O10 0.0380(12) 0.0565(13) 0.0605(14) 0.0001(11) 0.0062(10) -0.0051(10) O11 0.0586(18) 0.136(3) 0.0597(18) 0.0067(15) 0.0179(14) -0.0069(16) O12 0.0487(14) 0.0815(17) 0.0471(13) -0.0145(12) 0.0028(11) -0.0010(12) O13 0.0575(15) 0.0847(17) 0.0457(13) 0.0219(12) -0.0024(11) -0.0061(13) O14 0.0641(17) 0.0796(18) 0.0823(19) -0.0274(15) -0.0097(14) -0.0130(14) O15 0.0463(14) 0.0744(17) 0.0522(15) 0.0048(11) -0.0105(12) -0.0020(11) O16 0.083(2) 0.090(2) 0.102(2) 0.0405(18) -0.0160(18) 0.0200(17) O17 0.0392(12) 0.0747(16) 0.0604(15) 0.0051(12) 0.0042(11) 0.0094(11) O18 0.0370(12) 0.0465(12) 0.0373(12) 0.0035(8) -0.0012(9) -0.0008(8) N2 0.099(3) 0.100(3) 0.098(3) -0.0009(10) 0.0018(10) 0.0007(10) O19 0.127(3) 0.127(3) 0.126(3) -0.0013(10) 0.0024(10) -0.0014(10) O20 0.142(4) 0.143(4) 0.141(4) 0.0003(10) 0.0027(10) -0.0003(10) N2' 0.135(5) 0.136(5) 0.135(5) 0.0008(10) 0.0042(11) 0.0003(10) O19' 0.162(6) 0.162(6) 0.161(6) 0.0001(10) 0.0048(11) 0.0002(10) O20' 0.115(4) 0.114(4) 0.114(4) -0.0018(10) 0.0023(10) -0.0005(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.737(3) . ? Mo1 O17 1.903(2) . ? Mo1 O2 1.907(2) . ? Mo1 O3 1.979(2) . ? Mo1 O1 1.986(2) . ? Mo1 O18 2.2046(19) . ? Mo2 O4 1.681(3) . ? Mo2 O1 1.857(2) . ? Mo2 O7 1.893(3) . ? Mo2 O6 1.964(2) . ? Mo2 O5 1.969(2) . ? Mo2 O18 2.3259(19) . ? Mo3 O8 1.680(3) . ? Mo3 O3 1.869(2) . ? Mo3 O6 1.900(2) . ? Mo3 O9 1.955(2) . ? Mo3 O10 1.960(2) . ? Mo3 O18 2.331(2) . ? Mo4 O11 1.686(3) . ? Mo4 O13 1.884(3) . ? Mo4 O12 1.902(2) . ? Mo4 O17 1.946(2) . ? Mo4 O7 1.972(3) . ? Mo4 O18 2.324(2) . ? Mo5 O14 1.689(2) . ? Mo5 O15 1.895(2) . ? Mo5 O10 1.899(2) . ? Mo5 O2 1.930(2) . ? Mo5 O12 1.956(2) . ? Mo5 O18 2.3281(19) . ? Mo6 O16 1.679(3) . ? Mo6 O5 1.883(2) . ? Mo6 O9 1.889(2) . ? Mo6 O15 1.939(2) . ? Mo6 O13 1.954(3) . ? Mo6 O18 2.3745(19) . ? C1 N1 1.372(4) . ? C1 C6 1.383(5) . ? C1 C2 1.388(5) . ? C2 C3 1.380(6) . ? C2 C7 1.491(6) . ? C3 C4 1.369(9) . ? C3 H3 0.9300 . ? C4 C5 1.372(9) . ? C4 H4 0.9300 . ? C5 C6 1.355(7) . ? C5 N2' 1.408(8) . ? C5 N2 1.532(7) . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N3 1.524(6) . ? C8 C9 1.534(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.522(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.571(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.519(7) . ? C12 N3 1.527(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.503(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.474(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N3 1.515(5) . ? C16 C17 1.518(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.482(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.460(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N3 1.505(7) . ? C20 C21 1.541(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.480(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.502(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.485(6) . ? C24 N4 1.492(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.521(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.439(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.473(6) . ? C28 N4 1.525(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.548(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.493(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.498(7) . ? C32 N4 1.503(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.546(10) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.452(13) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.458(6) . ? C36 N4 1.541(5) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.555(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.462(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? N2 O20 1.275(7) . ? N2 O19 1.330(7) . ? N2' O19' 1.264(8) . ? N2' O20' 1.271(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 O17 103.18(13) . . ? N1 Mo1 O2 105.05(13) . . ? O17 Mo1 O2 90.74(10) . . ? N1 Mo1 O3 100.18(12) . . ? O17 Mo1 O3 156.23(10) . . ? O2 Mo1 O3 87.38(10) . . ? N1 Mo1 O1 98.33(12) . . ? O17 Mo1 O1 87.71(11) . . ? O2 Mo1 O1 156.29(10) . . ? O3 Mo1 O1 84.64(11) . . ? N1 Mo1 O18 175.27(12) . . ? O17 Mo1 O18 78.97(9) . . ? O2 Mo1 O18 79.02(8) . . ? O3 Mo1 O18 77.42(8) . . ? O1 Mo1 O18 77.46(9) . . ? O4 Mo2 O1 104.60(13) . . ? O4 Mo2 O7 104.88(14) . . ? O1 Mo2 O7 90.67(12) . . ? O4 Mo2 O6 102.08(13) . . ? O1 Mo2 O6 87.43(11) . . ? O7 Mo2 O6 152.56(10) . . ? O4 Mo2 O5 102.01(13) . . ? O1 Mo2 O5 153.02(10) . . ? O7 Mo2 O5 86.71(11) . . ? O6 Mo2 O5 82.78(10) . . ? O4 Mo2 O18 177.21(13) . . ? O1 Mo2 O18 76.91(9) . . ? O7 Mo2 O18 77.35(9) . . ? O6 Mo2 O18 75.56(8) . . ? O5 Mo2 O18 76.32(9) . . ? O8 Mo3 O3 104.52(13) . . ? O8 Mo3 O6 103.87(13) . . ? O3 Mo3 O6 89.97(11) . . ? O8 Mo3 O9 102.10(13) . . ? O3 Mo3 O9 153.23(10) . . ? O6 Mo3 O9 86.41(11) . . ? O8 Mo3 O10 103.16(13) . . ? O3 Mo3 O10 87.55(10) . . ? O6 Mo3 O10 152.60(10) . . ? O9 Mo3 O10 83.67(12) . . ? O8 Mo3 O18 178.92(13) . . ? O3 Mo3 O18 76.41(8) . . ? O6 Mo3 O18 76.61(9) . . ? O9 Mo3 O18 76.95(8) . . ? O10 Mo3 O18 76.28(8) . . ? O11 Mo4 O13 104.23(13) . . ? O11 Mo4 O12 103.38(13) . . ? O13 Mo4 O12 89.77(12) . . ? O11 Mo4 O17 102.90(13) . . ? O13 Mo4 O17 152.68(10) . . ? O12 Mo4 O17 87.05(11) . . ? O11 Mo4 O7 103.57(13) . . ? O13 Mo4 O7 86.41(11) . . ? O12 Mo4 O7 152.89(10) . . ? O17 Mo4 O7 84.22(11) . . ? O11 Mo4 O18 178.05(12) . . ? O13 Mo4 O18 77.66(9) . . ? O12 Mo4 O18 77.00(8) . . ? O17 Mo4 O18 75.18(8) . . ? O7 Mo4 O18 75.96(9) . . ? O14 Mo5 O15 103.16(13) . . ? O14 Mo5 O10 103.22(12) . . ? O15 Mo5 O10 88.88(11) . . ? O14 Mo5 O2 104.22(12) . . ? O15 Mo5 O2 152.47(10) . . ? O10 Mo5 O2 87.65(10) . . ? O14 Mo5 O12 103.39(12) . . ? O15 Mo5 O12 86.21(12) . . ? O10 Mo5 O12 153.36(10) . . ? O2 Mo5 O12 84.77(10) . . ? O14 Mo5 O18 179.26(11) . . ? O15 Mo5 O18 77.08(9) . . ? O10 Mo5 O18 77.47(8) . . ? O2 Mo5 O18 75.50(8) . . ? O12 Mo5 O18 75.91(8) . . ? O16 Mo6 O5 104.58(14) . . ? O16 Mo6 O9 104.12(14) . . ? O5 Mo6 O9 89.96(11) . . ? O16 Mo6 O15 103.54(14) . . ? O5 Mo6 O15 151.68(10) . . ? O9 Mo6 O15 86.38(12) . . ? O16 Mo6 O13 103.61(13) . . ? O5 Mo6 O13 86.42(11) . . ? O9 Mo6 O13 152.06(10) . . ? O15 Mo6 O13 83.86(12) . . ? O16 Mo6 O18 178.25(13) . . ? O5 Mo6 O18 76.66(9) . . ? O9 Mo6 O18 77.04(8) . . ? O15 Mo6 O18 75.15(9) . . ? O13 Mo6 O18 75.16(8) . . ? N1 C1 C6 117.7(4) . . ? N1 C1 C2 120.9(4) . . ? C6 C1 C2 121.4(4) . . ? C3 C2 C1 117.5(5) . . ? C3 C2 C7 122.6(5) . . ? C1 C2 C7 119.9(4) . . ? C4 C3 C2 121.6(6) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.2(5) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 121.5(6) . . ? C6 C5 N2' 137.4(8) . . ? C4 C5 N2' 100.7(8) . . ? C6 C5 N2 110.3(6) . . ? C4 C5 N2 128.2(7) . . ? N2' C5 N2 27.7(6) . . ? C5 C6 C1 118.9(5) . . ? C5 C6 H6 120.6 . . ? C1 C6 H6 120.6 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C9 114.5(4) . . ? N3 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N3 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 110.7(5) . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 C10 C11 114.2(8) . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N3 115.6(4) . . ? C13 C12 H12A 108.4 . . ? N3 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? N3 C12 H12B 108.4 . . ? H12A C12 H12B 107.4 . . ? C14 C13 C12 111.7(5) . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 113.5(7) . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 114.5(3) . . ? N3 C16 H16A 108.6 . . ? C17 C16 H16A 108.6 . . ? N3 C16 H16B 108.6 . . ? C17 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? C18 C17 C16 112.7(4) . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17B 109.0 . . ? C16 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C19 C18 C17 114.9(5) . . ? C19 C18 H18A 108.5 . . ? C17 C18 H18A 108.5 . . ? C19 C18 H18B 108.5 . . ? C17 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 115.7(5) . . ? N3 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? N3 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.4 . . ? C22 C21 C20 112.1(6) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C23 113.4(7) . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N4 118.4(4) . . ? C25 C24 H24A 107.7 . . ? N4 C24 H24A 107.7 . . ? C25 C24 H24B 107.7 . . ? N4 C24 H24B 107.7 . . ? H24A C24 H24B 107.1 . . ? C24 C25 C26 109.6(5) . . ? C24 C25 H25A 109.8 . . ? C26 C25 H25A 109.8 . . ? C24 C25 H25B 109.8 . . ? C26 C25 H25B 109.8 . . ? H25A C25 H25B 108.2 . . ? C27 C26 C25 115.4(7) . . ? C27 C26 H26A 108.4 . . ? C25 C26 H26A 108.4 . . ? C27 C26 H26B 108.4 . . ? C25 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N4 117.2(4) . . ? C29 C28 H28A 108.0 . . ? N4 C28 H28A 108.0 . . ? C29 C28 H28B 108.0 . . ? N4 C28 H28B 108.0 . . ? H28A C28 H28B 107.2 . . ? C28 C29 C30 110.1(4) . . ? C28 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? C28 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C29 114.6(4) . . ? C31 C30 H30A 108.6 . . ? C29 C30 H30A 108.6 . . ? C31 C30 H30B 108.6 . . ? C29 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 N4 117.7(4) . . ? C33 C32 H32A 107.9 . . ? N4 C32 H32A 107.9 . . ? C33 C32 H32B 107.9 . . ? N4 C32 H32B 107.9 . . ? H32A C32 H32B 107.2 . . ? C32 C33 C34 107.9(6) . . ? C32 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? C32 C33 H33B 110.1 . . ? C34 C33 H33B 110.1 . . ? H33A C33 H33B 108.4 . . ? C35 C34 C33 117.7(9) . . ? C35 C34 H34A 107.9 . . ? C33 C34 H34A 107.9 . . ? C35 C34 H34B 107.9 . . ? C33 C34 H34B 107.9 . . ? H34A C34 H34B 107.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 N4 116.6(4) . . ? C37 C36 H36A 108.1 . . ? N4 C36 H36A 108.1 . . ? C37 C36 H36B 108.1 . . ? N4 C36 H36B 108.1 . . ? H36A C36 H36B 107.3 . . ? C36 C37 C38 110.3(4) . . ? C36 C37 H37A 109.6 . . ? C38 C37 H37A 109.6 . . ? C36 C37 H37B 109.6 . . ? C38 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? C39 C38 C37 116.9(5) . . ? C39 C38 H38A 108.1 . . ? C37 C38 H38A 108.1 . . ? C39 C38 H38B 108.1 . . ? C37 C38 H38B 108.1 . . ? H38A C38 H38B 107.3 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C1 N1 Mo1 169.1(3) . . ? C20 N3 C16 111.4(4) . . ? C20 N3 C8 111.0(4) . . ? C16 N3 C8 106.5(3) . . ? C20 N3 C12 107.3(4) . . ? C16 N3 C12 110.3(4) . . ? C8 N3 C12 110.3(4) . . ? C24 N4 C32 105.6(3) . . ? C24 N4 C28 112.6(3) . . ? C32 N4 C28 110.7(3) . . ? C24 N4 C36 113.1(3) . . ? C32 N4 C36 111.9(3) . . ? C28 N4 C36 103.1(3) . . ? Mo2 O1 Mo1 114.46(12) . . ? Mo1 O2 Mo5 114.64(12) . . ? Mo3 O3 Mo1 114.88(11) . . ? Mo6 O5 Mo2 117.85(12) . . ? Mo3 O6 Mo2 117.38(11) . . ? Mo2 O7 Mo4 116.64(11) . . ? Mo6 O9 Mo3 117.31(11) . . ? Mo5 O10 Mo3 116.62(11) . . ? Mo4 O12 Mo5 116.90(11) . . ? Mo4 O13 Mo6 118.18(11) . . ? Mo5 O15 Mo6 118.57(13) . . ? Mo1 O17 Mo4 114.47(11) . . ? Mo1 O18 Mo4 91.21(7) . . ? Mo1 O18 Mo2 90.98(7) . . ? Mo4 O18 Mo2 90.04(7) . . ? Mo1 O18 Mo5 90.84(7) . . ? Mo4 O18 Mo5 89.95(7) . . ? Mo2 O18 Mo5 178.18(9) . . ? Mo1 O18 Mo3 91.28(7) . . ? Mo4 O18 Mo3 177.48(10) . . ? Mo2 O18 Mo3 90.31(7) . . ? Mo5 O18 Mo3 89.63(7) . . ? Mo1 O18 Mo6 179.75(11) . . ? Mo4 O18 Mo6 89.00(7) . . ? Mo2 O18 Mo6 89.17(6) . . ? Mo5 O18 Mo6 89.01(7) . . ? Mo3 O18 Mo6 88.51(7) . . ? O20 N2 O19 119.0(7) . . ? O20 N2 C5 116.2(7) . . ? O19 N2 C5 124.6(7) . . ? O19' N2' O20' 130.9(9) . . ? O19' N2' C5 123.3(11) . . ? O20' N2' C5 104.8(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C12 H12A O17 0.97 2.35 3.252(5) 154.2 . C28 H28B O12 0.97 2.53 3.287(5) 134.9 1_655 C29 H29A O6 0.97 2.42 3.344(5) 159.8 4_675 C24 H24A O6 0.97 2.48 3.332(5) 147.0 4_675 C37 H37A O5 0.97 2.47 3.302(5) 144.3 2_645 C24 H24B O4 0.97 2.51 3.437(5) 158.9 2_645 C28 H28B O12 0.97 2.53 3.287(5) 134.9 1_655 C16 H16B O15 0.97 2.45 3.143(5) 128.3 1_655 C10 H10B O8 0.97 2.55 3.359(8) 141.4 1_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.585 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.078